CN106483239A - A kind of detection method for producing short chain chlorinated paraffin in waste liquid - Google Patents
A kind of detection method for producing short chain chlorinated paraffin in waste liquid Download PDFInfo
- Publication number
- CN106483239A CN106483239A CN201510833034.3A CN201510833034A CN106483239A CN 106483239 A CN106483239 A CN 106483239A CN 201510833034 A CN201510833034 A CN 201510833034A CN 106483239 A CN106483239 A CN 106483239A
- Authority
- CN
- China
- Prior art keywords
- waste liquid
- hexane
- short chain
- detection method
- chlorinated paraffin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Abstract
A kind of detection method for producing short chain chlorinated paraffin in waste liquid, comprises the steps：（1）Sampling:In process of production, production waste liquid middle level liquid is taken, and 12-15 hour is incubated at 35-39 DEG C；（2）Sample pre-treatments:By step（1）Sample be placed in 50mL centrifuge tube, after adding 20mL n-hexane, it is vortexed on turbula shaker and mixes, under normal temperature after 260r/min mechanical shaking extraction 30min, 3000r/min is centrifuged 5min, take supernatant liquor to be transferred in 10mL centrifuge tube, at 40 DEG C, nitrogen blows evaporation and concentration near dry, is settled to 2mL with n-hexane；Purify again to be measured；（3）Detected using chromatograph.The present invention improves detection accuracy, reduces the error of detection, convenient operation.
Description
Technical field
The invention belongs to chemical technology field, specifically refers to a kind of detection method for producing short chain chlorinated paraffin in waste liquid.
Background technology
SCCPs（Short chain chlorinated paraffin）With thermally-stabilised, variable stickiness, good anti-flammability and insulating properties and low steam
The properties such as pressure.Which is mainly used as metal working lubricant, the fire retardant of textile and surface conditioning agent, fabric coating and leather
Plasticizer and fatting agent etc., are also used for the additive of rubber, paint, sealant, metal working fluid.SCCPs is mainly used by Switzerland
In joint sealant, in Korea, SCCPs is mainly used in the manufacture of lubricant and additive, Brazilian then be mainly used for SCCPs
Fire retardant in rubber, car carpeting and annex.The SCCPs of Canada, Australia and the state such as European Union is using being mainly used in gold
Category processing industry.China CPs is mainly used in PVC and rubber flame-retarded dose, lubrication oil coolant, oil paint additive and textile dyeing and finishing are helped
Agent field（Surface conditioning agent, the fire retardant of PVC coated fabric and plasticizer, leather fat as fabric and packaging）Deng use
Little in the amount of Metal Cutting.As China does not forbid the production of SCCPs and the content requirement of SCCPs in CPs is not had
Clear stipulaties, include the n-alkane that carbon chain lengths are for 10 ~ 13, so in the CPs product of China in the raw material of most of CPs
The overwhelming majority includes substantial amounts of SCCPs.
SCCPs stable chemical nature, does not specifically inhale color base group, under normal temperature under illumination of the wavelength more than 290nm
Photodissociation speed is slowly.The data display that European Union provides, SCCPs half-life in an atmosphere are 1.9 ~ 7.2 days, and
It is inversely proportional to carbon chain lengths.Under high latitude cryogenic conditions, aerosol has stronger suction-operated to SCCPs, may
Its oxidative pathway in an atmosphere can be limited.The research such as Madeley finds that SCCPs is degraded in nothing microorganism water environment
Possibility is less, and in having the environment of adapted microbes, chlorinity is relatively low（Chlorinity is less than 50%）SCCPs may
Slowly biodegradable, but most of SCCPs cannot then degrade.
Now, contain short chain chlorinated paraffin in the part Chemical Manufacture waste liquid of a lot of chlor-alkali production manufacturer production, without
Detection, and directly waste liquid is discharged, greatly destruction is caused to environment.
Therefore, a kind of detection method for producing short chain chlorinated paraffin in waste liquid of necessary design.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of detection method for producing short chain chlorinated paraffin in waste liquid.
Present invention employs technical scheme below,
A kind of detection method for producing short chain chlorinated paraffin in waste liquid, comprises the steps：
（1）Sampling
In process of production, production waste liquid middle level liquid is taken, and 12-15 hour is incubated at 35-39 DEG C；
（2）Sample pre-treatments
By step（1）Sample be placed in 50m L centrifuge tube, after adding 20m L n-hexane, be vortexed on turbula shaker mixed
Even, under normal temperature after 260 r/min mechanical shaking extraction, 30 min, 3000 r/min are centrifuged 5 min, take supernatant liquor and are transferred to
In 10 m L centrifuge tubes, at 40 DEG C, nitrogen blows evaporation and concentration near dry, is settled to 2 m L with n-hexane, to be clean；
Purify：Extracting solution carries out sulfonation with the concentrated sulfuric acid, until solution is transparent, then 3000 r/min are centrifuged 3min.Take 1m
Solution after L sulfonation, is transferred to preactivated florisil silica solid phase extraction column, with 2m L n-hexane drip washing, leacheate
Discard, with elution, eluent is collected, be blown to closely do through Nitrogen evaporator, n-hexane is settled to 1 m L redissolution, mixes, treats
Survey；
（3）Detected using chromatograph
Chromatographic condition is：ECD detector temperature：300℃；Injector temperature：280℃；Heating schedule：60 DEG C with 20 DEG C/
The ramp of min to 300 DEG C, keeps 12 min；Carrier gas：N2（Purity 99.999%）；1.0 m L/min of flow velocity；Enter
Sample amount：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Bushing pipe is not shunted using deactivation；FID detector temperature：
280℃；Injector temperature：280℃；Heating schedule：50 DEG C of initial temperature, with 10 DEG C/min ramp to 240 DEG C, keeps
4 min；Carrier gas：H2（Purity 99.999%）, 2 m L/min of flow；Combustion gas：H2,30 m L/min of flow, combustion-supporting gas：
Air, 300 m L/min of flow；Sample size：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Using filling
The deactivation of palladium catalyst does not shunt bushing pipe.
In the present invention, as a kind of preferred technical scheme, when the concentrated sulfuric acid carries out sulfonation, concentrated sulfuric acid usage amount is 2 m L/
Secondary.
In the present invention, as a kind of preferred technical scheme, all containers are all carried out clearly with dichloromethane before and after use
After washing twice, it is put in Muffle furnace 400 DEG C and dries 6 hours, using deionized water cleaning, drying after taking-up.
In the present invention, used as a kind of preferred technical scheme, solid-phase extraction device extraction core is clear using organic solvent ultrasound
Dry after washing three times, every group of sample 10 additions, one blank sample is in order to check the dirt being likely to occur in pretreatment process
Dye.
In the present invention, as a kind of preferred technical scheme, eluent is the mixture of n-hexane and ethyl acetate.
In the present invention, used as a kind of preferred technical scheme, the volume ratio of n-hexane and ethyl acetate is 1：3.
The invention has the beneficial effects as follows,
The present invention improves detection accuracy, reduces the error of detection, convenient operation.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
A kind of detection method for producing short chain chlorinated paraffin in waste liquid, comprises the steps：
（1）Sampling
In process of production, production waste liquid middle level liquid is taken, at 39 DEG C, is incubated 15 hours；
（2）Sample pre-treatments
By step（1）Sample be placed in 50m L centrifuge tube, add 20m L n-hexane after, on turbula shaker be vortexed
Mix, under normal temperature after 260 r/min mechanical shaking extraction, 30 min, 3000 r/min are centrifuged 5 min, take supernatant liquor transfer
To 10 m L centrifuge tubes, at 40 DEG C, nitrogen blows evaporation and concentration near dry, is settled to 2 m L with n-hexane, to be clean；
Purify：Extract the solution concentrated sulfuric acid（2 m L/ time）Carry out sulfonation, until solution is transparent, then 3000 r/min from
Heart 3min.Take the solution after 1m L sulfonation, be transferred to preactivated florisil silica solid phase extraction column, with 2m L just oneself
Alkane drip washing, leacheate are discarded, and with elution, eluent is the mixture of n-hexane and ethyl acetate, n-hexane and acetic acid
The volume ratio of ethyl ester is 1：3, eluent to be collected, is blown to closely do through Nitrogen evaporator, n-hexane is settled to 1 m L redissolution, mixes, treats
Survey；
（3）Detected using chromatograph
Chromatographic condition is：ECD detector temperature：300℃；Injector temperature：280℃；Heating schedule：60 DEG C with 20 DEG C/
The ramp of min to 300 DEG C, keeps 12 min；Carrier gas：N2（Purity 99.999%）；1.0 m L/min of flow velocity；Enter
Sample amount：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Bushing pipe is not shunted using deactivation；FID detector temperature：
280℃；Injector temperature：280℃；Heating schedule：50 DEG C of initial temperature, with 10 DEG C/min ramp to 240 DEG C, keeps
4 min；Carrier gas：H2（Purity 99.999%）, 2 m L/min of flow；Combustion gas：H2,30 m L/min of flow, combustion-supporting gas：
Air, 300 m L/min of flow；Sample size：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Using filling
The deactivation of palladium catalyst does not shunt bushing pipe.
In the present invention, after all containers are all carried out twice with dichloromethane before and after use, it is put in Muffle furnace
400 DEG C are dried 6 hours, using deionized water cleaning, drying after taking-up.
In the present invention, solid-phase extraction device extraction core using organic solvent be cleaned by ultrasonic three times after dry, every group of sample 10
One blank sample of individual addition is in order to check the pollution being likely to occur in pretreatment process.
1 test result of embodiment is as follows：
Embodiment 2
A kind of detection method for producing short chain chlorinated paraffin in waste liquid, comprises the steps：
（1）Sampling
In process of production, production waste liquid middle level liquid is taken, at 35 DEG C, is incubated 12 hours；
（2）Sample pre-treatments
By step（1）Sample be placed in 50m L centrifuge tube, after adding 20m L n-hexane, be vortexed on turbula shaker mixed
Even, under normal temperature after 260 r/min mechanical shaking extraction, 30 min, 3000 r/min are centrifuged 5 min, take supernatant liquor and are transferred to
In 10 m L centrifuge tubes, at 40 DEG C, nitrogen blows evaporation and concentration near dry, is settled to 2 m L with n-hexane, to be clean；
Purify：Extract the solution concentrated sulfuric acid（2 m L/ time）Sulfonation is carried out, until solution is transparent, then 3000 r/min centrifugation
3min.The solution after 1m L sulfonation is taken, preactivated florisil silica solid phase extraction column is transferred to, with 2m L n-hexane
Drip washing, leacheate are discarded, and with elution, eluent is the mixture of n-hexane and ethyl acetate, n-hexane and acetic acid second
The volume ratio of ester is 1：3, eluent to be collected, is blown to closely do through Nitrogen evaporator, n-hexane is settled to 1 m L redissolution, mixes, treats
Survey；
（3）Detected using chromatograph
Chromatographic condition is：ECD detector temperature：300℃；Injector temperature：280℃；Heating schedule：60 DEG C with 20 DEG C/
The ramp of min to 300 DEG C, keeps 12 min；Carrier gas：N2（Purity 99.999%）；1.0 m L/min of flow velocity；Enter
Sample amount：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Bushing pipe is not shunted using deactivation；FID detector temperature：
280℃；Injector temperature：280℃；Heating schedule：50 DEG C of initial temperature, with 10 DEG C/min ramp to 240 DEG C, keeps
4 min；Carrier gas：H2（Purity 99.999%）, 2 m L/min of flow；Combustion gas：H2,30 m L/min of flow, combustion-supporting gas：
Air, 300 m L/min of flow；Sample size：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Using filling
The deactivation of palladium catalyst does not shunt bushing pipe.
Those of ordinary skill in the art should be understood：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, step can be realized with random order, and is existed such as
Many other changes of the different aspect of the upper described present invention, for their not offers in details simple and clear.Therefore, all
Within the spirit and principles in the present invention, any omission for being made, modification, equivalent, improvement etc., should be included in the present invention's
Within protection domain.
Claims (6)
1. a kind of detection method for producing short chain chlorinated paraffin in waste liquid, is characterized in that, comprise the steps：
（1）Sampling
In process of production, production waste liquid middle level liquid is taken, and 12-15 hour is incubated at 35-39 DEG C；
（2）Sample pre-treatments
By step（1）Sample be placed in 50m L centrifuge tube, add 20m L n-hexane after, on turbula shaker be vortexed
Mix, under normal temperature after 260 r/min mechanical shaking extraction, 30 min, 3000 r/min are centrifuged 5 min, take supernatant liquor transfer
To 10 m L centrifuge tubes, at 40 DEG C, nitrogen blows evaporation and concentration near dry, is settled to 2 m L with n-hexane, to be clean；
Purify：Extracting solution carries out sulfonation with the concentrated sulfuric acid, until solution is transparent, then 3000 r/min are centrifuged 3min,
The solution after 1m L sulfonation is taken, preactivated florisil silica solid phase extraction column is transferred to, with 2m L n-hexane
Drip washing, leacheate are discarded, and with elution, collect eluent, are blown to closely do through Nitrogen evaporator, and n-hexane is settled to 1 m L
Redissolve, mix, to be measured；
（3）Detected using chromatograph
Chromatographic condition is：ECD detector temperature：300℃；Injector temperature：280℃；Heating schedule：60 DEG C with 20 DEG C/
The ramp of min to 300 DEG C, keeps 12 min；Carrier gas：N2（Purity 99.999%）；1.0 m L/min of flow velocity；Enter
Sample amount：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Bushing pipe is not shunted using deactivation；FID detector temperature：
280℃；Injector temperature：280℃；Heating schedule：50 DEG C of initial temperature, with 10 DEG C/min ramp to 240 DEG C, keeps
4 min；Carrier gas：H2（Purity 99.999%）, 2 m L/min of flow；Combustion gas：H2,30 m L/min of flow, combustion-supporting gas：
Air, 300 m L/min of flow；Sample size：1 µL；Input mode：Do not shunt, valve opening after 0.75 min；Using filling
The deactivation of palladium catalyst does not shunt bushing pipe.
2. a kind of detection method for producing short chain chlorinated paraffin in waste liquid as claimed in claim 1, is characterized in that, the concentrated sulfuric acid enters
During row sulfonation, concentrated sulfuric acid usage amount is 2 m L/ time.
3. a kind of detection method for producing short chain chlorinated paraffin in waste liquid as claimed in claim 1, is characterized in that, all containers
After being all carried out twice with dichloromethane before and after use, it is put in Muffle furnace 400 DEG C and dries 6 hours, using goes after taking-up
Ionized water cleaning, drying.
4. a kind of detection method for producing short chain chlorinated paraffin in waste liquid as claimed in claim 1, is characterized in that, SPE
Device extraction core is cleaned by ultrasonic after three times using organic solvent and dries, and 10, every group of sample adds a blank sample in order to examine
Look into the pollution being likely to occur in pretreatment process.
5. a kind of detection method for producing short chain chlorinated paraffin in waste liquid as claimed in claim 1, is characterized in that, eluent is
N-hexane and the mixture of ethyl acetate.
6. a kind of detection method for producing short chain chlorinated paraffin in waste liquid as claimed in claim 1, is characterized in that, n-hexane and
The volume ratio of ethyl acetate is 1：3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510833034.3A CN106483239A (en) | 2015-11-25 | 2015-11-25 | A kind of detection method for producing short chain chlorinated paraffin in waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510833034.3A CN106483239A (en) | 2015-11-25 | 2015-11-25 | A kind of detection method for producing short chain chlorinated paraffin in waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106483239A true CN106483239A (en) | 2017-03-08 |
Family
ID=58238540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510833034.3A Pending CN106483239A (en) | 2015-11-25 | 2015-11-25 | A kind of detection method for producing short chain chlorinated paraffin in waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106483239A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109142555A (en) * | 2018-05-21 | 2019-01-04 | 深圳天祥质量技术服务有限公司 | The test method of MCCP in plastics or leather and fur products |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04157955A (en) * | 1990-10-22 | 1992-05-29 | Nec Corp | Protocol processing method for signal connection control part of no.7 signal system |
| US5721728A (en) * | 1995-12-21 | 1998-02-24 | Lucent Technologies Inc. | Network node testing method and apparatus |
| CN102507783A (en) * | 2011-11-10 | 2012-06-20 | 深圳天祥质量技术服务有限公司 | Method for detecting short-chain chlorinated paraffins (SCCPs) |
| CN103012050A (en) * | 2011-09-21 | 2013-04-03 | 中国科学院大连化学物理研究所 | Synthesizing method of polychloroalkane |
-
2015
- 2015-11-25 CN CN201510833034.3A patent/CN106483239A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04157955A (en) * | 1990-10-22 | 1992-05-29 | Nec Corp | Protocol processing method for signal connection control part of no.7 signal system |
| US5721728A (en) * | 1995-12-21 | 1998-02-24 | Lucent Technologies Inc. | Network node testing method and apparatus |
| CN103012050A (en) * | 2011-09-21 | 2013-04-03 | 中国科学院大连化学物理研究所 | Synthesizing method of polychloroalkane |
| CN102507783A (en) * | 2011-11-10 | 2012-06-20 | 深圳天祥质量技术服务有限公司 | Method for detecting short-chain chlorinated paraffins (SCCPs) |
Non-Patent Citations (1)
| Title |
|---|
| 史惠娟等: "快速溶剂萃取-气相色谱法测定油漆中的短链氯化石蜡", 《山西大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109142555A (en) * | 2018-05-21 | 2019-01-04 | 深圳天祥质量技术服务有限公司 | The test method of MCCP in plastics or leather and fur products |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ma et al. | Determination of endocrine-disrupting compounds in water by carbon nanotubes solid-phase microextraction fiber coupled online with high performance liquid chromatography | |
| CN107290316B (en) | Novel tetracycline fluorescence detection method based on zirconium-based MOF | |
| CN103816877B (en) | A kind of solid phase micro extraction probe and its preparation method and application | |
| Zeng et al. | Development of polymethylphenylsiloxane-coated fiber for solid-phase microextraction and its analytical application of qualitative and semi-quantitative of organochlorine and pyrethroid pesticides in vegetables | |
| Li et al. | Characterization of polycyclic aromatic hydrocarbons in fog–rain events | |
| CN106345800B (en) | Method for removing polycyclic aromatic hydrocarbons in soil by persulfate-calcium peroxide composite oxidation | |
| CN101122588A (en) | Method for determining polycyclic aromatic hydrocarbons in sludge | |
| CN104698109B (en) | The detection method of phthalate plasticiser in a kind of edible oil | |
| CN108008029A (en) | The dispersive solid-phase extraction of Phthalates of Environment Hormone-gas chromatography-mass spectrum detection method in a kind of marine sediment | |
| CN103776924A (en) | Method for detecting polycyclic aromatic hydrocarbon in fried food | |
| CN104193875B (en) | The preparation method of stilboestrol magnetic molecularly imprinted polymer and application thereof | |
| CN104568562A (en) | Water sample and pretreatment method of nitrosoamine compound in suspended matter of water sample | |
| CN106483239A (en) | A kind of detection method for producing short chain chlorinated paraffin in waste liquid | |
| Li et al. | Liquid-phase deposition of silica nanoparticles into a capillary for in-tube solid-phase microextraction coupled with high-performance liquid chromatography | |
| CN105699526A (en) | Method for detecting contents of brominated flame retardant and phosphorus-based flame retardant in hairs | |
| CN110412169A (en) | The on-line solid phase extraction gaschromatographic mass spectrometry detection method of organotin in marine sediment | |
| CN107202854B (en) | A kind of method of polybrominated diphenyl ether residue amount in quick detection shellfish | |
| CN104353441B (en) | A kind of ion blotting material for enrichment water body ultra trace methyl mercury | |
| CN106033080A (en) | Rapid detection method for detecting multiple residual pesticides in edible plant oil and pretreatment method thereof | |
| CN111085006A (en) | Process for extracting organic pollutants in environment | |
| CN108414637B (en) | Method for detecting volatile disinfection byproducts in water by utilizing solid phase microextraction-gas chromatography-mass spectrometry combined technology | |
| CN104458935A (en) | Method for detecting plasticizer in Baijiu | |
| CN105424459B (en) | A kind of absorptive element and solid-phase micro-extracting device | |
| CN104991012B (en) | Sample purifying device capable of separating HBCDs and TBBPA simultaneously | |
| CN108152281A (en) | A kind of chitosan solution is modified method for preparing test paper |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170308 |