CN105834177A - Acid pickling method for plastic sample bottles - Google Patents
Acid pickling method for plastic sample bottles Download PDFInfo
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- CN105834177A CN105834177A CN201610321994.6A CN201610321994A CN105834177A CN 105834177 A CN105834177 A CN 105834177A CN 201610321994 A CN201610321994 A CN 201610321994A CN 105834177 A CN105834177 A CN 105834177A
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- bottle
- sample bottles
- sample bottle
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- pickling
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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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- Mechanical Engineering (AREA)
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Abstract
The invention discloses an acid pickling method for plastic sample bottles. The acid pickling method for the plastic sample bottles comprises the following steps: filling a 100-level ultra-clean bench with 5-10% of a nitric acid solution prepared from Milli-Q ultra-pure water; rotating bottle bodies to remove air bubbles on bottle walls and in an acid pickling solution and enabling the sample bottles to be upright; packaging the sample bottles in a sealed manner by using double-layered plastic bags which are clean after being subjected to acid pickling; standing for 30-60 days at normal temperature and always keeping the sample bottles upright; pouring out the first-time acid pickling solution from the 100-level ultra-clean bench; washing the 100-level ultra-clean bench for 3 times by using the Milli-Q ultra-pure water; filling the 100-level ultra-clean bench with 0.1-0.5% of a high-purity nitric acid solution prepared from the Milli-Q ultra-pure water; rotating the bottle bodies to remove the air bubbles on the bottle walls and in the acid pickling solution and enabling the sample bottles to be upright; packaging the sample bottles in a sealed manner by using the double-layered plastic bags which are clean after being subjected to acid pickling; keeping the sample bottles upright and standing for 2 months at normal temperature; and continuing placing the sample bottles subjected to acid pickling for the second time in the original packages for 1-12 months until the sample bottles are used and then 'ageing' the sample bottles by using the nitric acid solution. A blank check shows that the acid pickling method disclosed by the method is effective.
Description
Technical field
The present invention relates to the acid washing method of a kind of plastic sample bottle, refer specifically to pouring-in acid washing method.
Background technology
In mountain region and polar region snow ice, the concentration of trace element is the lowest, from the collection of sample, transports, is stored to last point
During analysis, all plastic sample bottles directly contacted with sample can be by the direct contaminated samples of dissolution trace element.Therefore need
Use suitable acid washing method that plastic sample bottle is carried out, to reduce plastic sample bottle bottle to greatest extent to snow ice sample
The pollution of product.Existing plastic sample bottle pickling is, in four time-of-weeks, plastic sample bottle is immersed in first to fourth successively
In the salpeter solution of acid wash drum, the concentration of salpeter solution is sequentially reduced and purity is gradually increased；Except first pass pickling is in room temperature
Under carry out beyond, rear three times pickling all be with heater plate with accelerate pickling process.Existing acid washing method cleans journey
Sequence is complicated, inefficient, expends substantial amounts of manpower, also easily causes security incident, and its main not enough performance is as follows:
1. acid cleaning process is the soak acid-cleaning utilizing 4 acid wash drums to carry out successively 4 weeks, because of the finite capacity of acid wash drum, and a collection of
A small amount of sample bottle can be cleaned, it is impossible to meet the demand of Ice core study sample bottle clean to a large amount of pickling.
2. complicated, the pickling process of pipeline system needs special messenger to carry out weekly continual cleaning guarantee acid dip pickle
Recycle.Additionally, the transfer that sample bottle is between 4 acid wash drums needs to expend substantial amounts of people with up to ten flushings several times
Power, has had a strong impact on the efficiency of pickling.
3., due to the effect of buoyancy, sample segment bottle swims in acid wash drum and sample bottle cannot be made above pickle complete
Complete immersion is in pickle, it is impossible to ensure effective pickling of sample bottle.Additionally, due to the bubble being attached to bottle wall cannot be removed,
Cause sample bottle bottle wall not to be fully contacted with pickle, also have impact on the effect of pickling.
4. it is the heater plate by bottom due to acid wash drum, easily sends out when heating plate temperature-controlling system breaks down
Coin into acid wash drum high temperature melting and the security incident of pickle leakage.
Summary of the invention
In view of above-mentioned, it is an object of the invention to the acid washing method by direct injection and complete the clear of plastic sample bottle
Washing, pickling process is easier, efficient, it is ensured that pickle and sample bottle inwall are fully contacted and effectively pickling, greatly reduce
Work is time-consuming, can meet trace element research to the demand of a large amount of clean sample bottles the generation that reduces security incident.
The object of the present invention is achieved like this:
A kind of acid washing method of plastic sample bottle, its step includes:
A, first pass pickling:
It is 100 grades of superclean benches at ultra-clean Cleanliness, opens bottle cap, fill with the BV-III level nitre of secondary sub-boiling distillation
(Beijing Inst. of Chemical Reagent, with Determination of trace element contents for 10 in acid-9G/g magnitude) and Milli-Q ultra-pure water (resistivity is
18.2 M Ω .cm) prepare 5 ~ 10% salpeter solution.Cover bottle cap, tilt and rotate bottle, allow in bottle wall and pickle
Bubble is fused into large volume of bubble and rises to liquid level and rupture, and then sample bottle is uprightly put into clean low of double-deck pickling
Density polyethylene plastic bag carries out packaging seal, and (more than 20 DEG C) stand 30 ~ 60 days at normal temperatures, and period is at Low Density Polyethylene
The erectility of sample bottle is remained in plastic bag；
B, washing:
In clean room, sample bottle upright in taking out LDPE: Low-density polyethylene plastics bag, open bottle cap, first pass pickle is fallen
Go out, with Milli-Q ultra-pure water, plastic sample bottle is rinsed 3 times, rinse out the first pass acid of plastic sample bottle surface attachment completely
Washing liquid；
C, second time pickling:
Bottle cap opened by superclean bench in clean room, fills with Fiher " Optima " level high-purity concentrated nitric acid (trace element
Content is 10-12G/g magnitude) and Milli-Q ultra-pure water prepare 0.1 ~ 0.5% salpeter solution, cover bottle cap, tilt and revolve
Rolling bottle body, allows the bubble in bottle wall and pickle be fused into large volume of bubble and to rise to liquid level and rupture, then sample
Bottle is uprightly put into the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling and is carried out packaging seal, and (more than 20 DEG C) stand at normal temperatures
2 months, period remained the erectility of sample bottle；
D, " aging " of salpeter solution:
Sample bottle after second time pickling is continued placement 1 ~ 12 month in original packing, until before Shi Yonging, carrying out salpeter solution
" aging " effect, with the trace element of dissolution bottle to greatest extent；
E, blank check:
Randomly draw washed sample bottle, inject Milli-Q ultra-pure water about 30 mL and with high pure nitric acid (Fisher
" Opitima " level nitric acid) acidifying is 1%, at room temperature stands after 48 hours by Finnigan MAT Element inductive etc.
Gas ions mass spectrograph (power & light company of the U.S.) measures, test result display the tested main trace element Al of all samples, Mn,
The concentration of Fe, Co, Cu, Zn, Sr, Sb, Cs, Ba, Tl, Pb and Bi below detects limit, or not detection.Show direct injection
Acid washing method is effective, is suitable for snow and ice and other environmental sample trace element analysis.
The invention have the advantage that
1. need not to utilize acid wash drum to carry out soak acid-cleaning, acid and alkali cask washing holds quantitative limitation, the most a collection of can be appropriate with pickling
Sample bottle, so can meet the demand of sample bottle clean to a large amount of pickling.
2. direct injection acid washing method simplifies pickling process, greatly reduce sample bottle shift between acid wash drum and
The number of times rinsed, it is not necessary to special messenger carries out weekly routine cleaning, it is to avoid numerous and diverse workload of knowing clearly, and improves the efficiency of pickling.
3. sample bottle has filled pickle, remains that level uprightly stands shape after getting rid of the bubble in bottle wall and pickle
State, can make sample bottle bottle inwall be fully contacted with pickle, the effect of know clearly pickling is effectively ensured.
The most pouring-in acid washing method can allow sample bottle be full of second time pickle and place for a long time, this salpeter solution
" aging " effect can the trace element in dissolution bottle to greatest extent, significantly reduce blank, it is to avoid the pollution to sample.
5. the pouring-in acid cleaning process of sample bottle is all carried out at superclean bench, so can avoid room air pair
The pollution of sample bottle, it is ensured that the effectiveness of pickling.
The most all of pickling process carries out the most at normal temperatures, it is not necessary to use heating plate to heat, it is to avoid acid
The security incident that cask washing high temperature melting and pickle are revealed.
Detailed description of the invention
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 includes:
A, first pass pickling:
Staff dresses clean clothing, mask and disposable Low Density Polyethylene glove 10000 grades of clean room 100 grades
Open bottle cap in superclean bench, fill 5 ~ 10% salpeter solutions with the configuration of Milli-Q ultra-pure water, screw bottle cap.High-purity nitre
The BV-III level nitric acid that acid is produced by Beijing Inst. of Chemical Reagent in advance is prepared by the method for secondary sub-boiling distillation further.
Then cover bottle cap, tilt with hands and rotate bottle gently, allow the minute bubbles being attached on bottle wall depart from bottle wall and pickle
In other bubble collide with each other and form bigger bubble, relief its rise to pickling liquid level and rupture, so can ensure that
Pickle is fully contacted with bottle inwall.After getting rid of bubble, sample bottle is uprightly placed on desktop, fills all of sample according to this
Bottle, is then kept upright sample bottle and puts the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling into and seal.Finally will
Plastic packaging bag equipped with sample bottle is placed in parallel on the rack in clean room and remains the erectility of sample bottle,
(more than 20 DEG C) stand 30 ~ 60 days at normal temperatures；
B, washing:
Superclean bench in clean room, has taken out the sample bottle of for the first time pickling, has opened bottle cap from plastic packaging bag, by the
One time pickle is poured out, and with Milli-Q ultra-pure water rinsing 3 times inside and outside plastic sample bottle bottle and bottle cap, rinses out mould completely
The first pass pickle of material sample bottle surface attachment；
C, second time pickling:
0.1 ~ 0.5% Fisher " Optima " the level high pure nitric acid with the configuration of Milli-Q ultra-pure water is filled in superclean bench
Solution, screws bottle cap.Method during same use pickling for the first time gets rid of the bubble in bottle wall and pickle, then sample bottle
It is kept upright and puts the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling into and seal.Finally will be equipped with the plastics of sample bottle
Packaging bag is placed in parallel on the rack in clean room and remains the erectility of sample bottle, at normal temperatures (20 DEG C with
On) stand 2 months；
D, " aging " of salpeter solution:
Sample bottle after second time pickling is continued in original packaging placement 1 ~ 12 month even more long-time until using
Before, carry out " aging " effect of salpeter solution, with the trace element of dissolution bottle to greatest extent, reduce the blank of sample bottle,
Reduce the pollution to sample；
E, blank check:
In order to check the effectiveness of the pouring-in acid washing method of the present invention, the sample bottle of pickling is carried out blank determination.Take out at random
Take the washed sample bottle of 8 30 mL, inject Milli-Q ultra-pure water about 30 mL and by high pure nitric acid (Fisher " Opitima " level
Nitric acid) acidifying is 1%, at room temperature stands after 48 hours with Finnigan MAT Element inductivity coupled plasma mass spectrometry
Instrument (power & light company of the U.S.) measures at 100 grades of laminar flow superclean benches.The test result display tested main trace of all samples
The concentration of secondary element Al, Mn, Fe, Co, Cu, Zn, Sr, Sb, Cs, Ba, Tl, Pb and Bi below detects limit, not detection.Test
The detection limit of method is molten using 1% nitric acid (by Milli-Q water-reducible Fisher " Opitima " level salpeter solution) as blank
Liquid METHOD FOR CONTINUOUS DETERMINATION 10 times, calculates the standard deviation δ of 10 measured values, using concentration corresponding to the standard deviations of 3 times (3 δ) as side
The detection limit of method.The above each Element detection limit calculated by the 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 and Bi 0.05.Table
The direct injection acid washing method of the bright present invention is effective, is suitable for snow and ice and other environmental sample trace element divides
Analysis.
Second time pickle is poured out before using by sample bottle at superclean bench, with Milli-Q ultrapure water 3 times, dries in the air
Dry standby.
Claims (1)
1. an acid washing method for plastic sample bottle, its step includes:
A, first pass pickling:
It is 100 grades of superclean benches at ultra-clean Cleanliness, opens bottle cap, fill with the BV-III level nitre of secondary sub-boiling distillation
Acid and Milli-Q ultra-pure water prepare 5 ~ 10% salpeter solution；Cover bottle cap, tilt and rotate bottle, allow bottle wall and pickling
Bubble in liquid is fused into large volume of bubble and rises to liquid level and rupture, and then sample bottle is uprightly put into double-deck pickling and does
Clean LDPE: Low-density polyethylene plastics bag carries out packaging seal, stands 30 ~ 60 days at normal temperatures, and period is at LDPE: Low-density polyethylene plastics
The erectility of sample bottle is remained in Dai；
B, washing:
In clean room, sample bottle upright in taking out LDPE: Low-density polyethylene plastics bag, open bottle cap, first pass pickle is fallen
Go out, with Milli-Q ultra-pure water, plastic sample bottle is rinsed 3 times, rinse out the first pass acid of plastic sample bottle surface attachment completely
Washing liquid；
C, second time pickling:
Bottle cap opened by superclean bench in clean room, fills and surpasses with Fiher " Optima " level high pure nitric acid and Milli-Q
The salpeter solution of the 0.1 ~ 0.5% of pure water preparation, covers bottle cap, tilts and rotates bottle, allows the bubble in bottle wall and pickle melt
Synthesizing large volume of bubble and rise to liquid level and rupture, the low-density then sample bottle uprightly being put into double-deck pickling clean is gathered
Vinyl bag carries out packaging seal, stands 2 months at normal temperatures, and period remains the erectility of sample bottle；
D, " aging " of salpeter solution:
Sample bottle after second time pickling is continued placement 1 ~ 12 month in original packing, until before Shi Yonging, carrying out salpeter solution
" aging " effect, with the trace element of dissolution bottle to greatest extent；
E, blank check
Randomly draw washed sample bottle, inject Milli-Q ultra-pure water about 30 mL and be 1% with high pure nitric acid acidifying, in room temperature
Lower standing was carried out with Finnigan MAT Element icp ms (power & light company of the U.S.) after 48 hours
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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105834177A true CN105834177A (en) | 2016-08-10 |
| CN105834177B CN105834177B (en) | 2017-12-08 |
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ID=56592383
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2016
- 2016-05-16 CN CN201610321994.6A patent/CN105834177B/en not_active Expired - Fee Related
Patent Citations (5)
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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 |
| JP2016016354A (en) * | 2014-07-08 | 2016-02-01 | 三菱重工食品包装機械株式会社 | Barrier thin film post-processing method, and cleaning device |
| CN105057271A (en) * | 2015-07-17 | 2015-11-18 | 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 |
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| 刘亚平等: "极地雪冰样品超痕量重金属分析", 《冰川冻土》 * |
Cited By (1)
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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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| Publication number | Publication date |
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| CN105834177B (en) | 2017-12-08 |
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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 |