CN103439476B - Turnover testing device and method for heavy metal availability by stimulating human digestion characteristics - Google Patents
Turnover testing device and method for heavy metal availability by stimulating human digestion characteristics Download PDFInfo
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Abstract
The invention provides a turnover testing device and method for heavy metal availability by stimulating human digestion characteristics. The method comprises the following steps of: (1) preprocessing a soil sample; (2) preparing simulated gastric fluid and intestinal fluid and heating; (3) simultaneously adding the preprocessed soil sample and the simulated gastric fluid into an extraction bottle and regulating the pH of the solution; (4) continuously overturning and oscillating; (5) at the end of oscillation, filtering with a filtering membrane, and analyzing the human availability of the heavy metal in a stomach stage by utilizing an ICP-MS (Inductively Coupled Plasma Mass Spectrometry); (6) after supplementing the fresh gastric fluid, adding the simulated gastric fluid, regulating the pH, and fixing the solution into an extraction chamber; (7) overturning and oscillating; (8) at the end of oscillation, filtering with the mixture to pass through the filtering membrane, and analyzing the human availability of the heavy metal in an intestine stomach stage by utilizing the ICP-MS. The testing method provided by the invention is simple in operation and large in testing capacity, requires few instruments, is capable of realizing automatic control and simultaneously testing 12 samples and can be widely used for testing the human availability of soil heavy metal in polluted sites.
Description
Technical field
The invention belongs to the field of Environment Protection of contaminated site health test, particularly relate to a kind of human intestines and stomach of simulation and digest the heavy metal in soil human body of feature to the convertible Test integration device and method of property.
Background technology
Because environmental practice is not in place in smelting in early days, metallic article (as plating, the casting) production run such as processing and manufacturing, chromic salts, soil within the scope of these plant areas of enterprise is caused to be subject to heavy metal pollution.Carry out place assessment discovery as moved certain chemical plant to Beijing, plant area's As, Hg, Cr contaminated soil reaches 3.1 ten thousand m
3.Carry out assessment to dyestuff factory, Beijing soil to find, As, Cr contaminated soil reaches 5.2 ten thousand m
3.Carry out assessment to discarded dyestuff factory, Wuhan to find, As contaminated soil reaches 18.4 ten thousand m
3.Affect by the blowdown of Zhuzhou Deng Di smelting enterprise, the By The Heavy Metal Contaminated Soil in whole Hunan Province nearly 13%, reaches 28000 hm2.Carry out assessment to plant area of former Changsha Chromates Plant soil to find, this plant area needs the Cr contaminated soil repaired to reach 200,000 m
3.By in September, 2011, Pengzhou, Sichuan determines 15 pieces of heavy metal pollution places by risk assessment.
For meeting town site demand, these heavy industries contaminated site land character often will change business or residential estate into.For guaranteeing the health of the rear following use crowd of this kind of place redevelopment, need assess heavy metal pollution degree in the soil of place and take corresponding risk control measure according to result.Wherein, based on human healthy risk assessment's result formulate corresponding risk management and control measure accept by environmental administration at different levels.At present when carrying out heavy metal pollution of soil risk assessment, because hypothesis heavy metal in soil is taken in after human body with soil per os can be entered blood circulation of human body system completely and work the mischief to human body, when calculating reconditioning generally with heavy metal in soil total amount for benchmark.But increasing research shows, even if under the gastric fluid conditions of extreme acidic, heavy metal also can not dissolve completely and enter in human gastric juice from soil.Therefore, adopt that to carry out assessing obtained result with heavy metal in soil total amount very conservative, cause huge sum of money contaminated soil excessively to be repaired, waste unnecessary reparation fund.
Carry out assessing the problem causing result too to be guarded based on heavy metal in soil total amount at present for overcoming, the most effective approach is the biological effectiveness (i.e. in-vivo test) adopting heavy metal in animal toxicity test testing soil.But, this method often consuming time longer, cost is higher, simultaneously because of using animal as tested donor, ethics endures dispute to the fullest extent always.The prerequisite being rapidly absorbed into blood circulation of human body system due to heavy metal in soil is that it desorb can enter the gastronintestinal system of human body from soil, and large quantity research shows, the amount being dissolved in pollutant in human intestines and stomach's system and the final measurer entered in blood circulation system have good correlativity, the exposed amount as human body that can guard.Therefore, the in-vitro simulated method of testing (i.e. in-vitro test) extracted pollutant in soil for extraction agent with human stomach intestinal juice progressively replaces the complicated in-vivo test of tradition and can test to property for heavy metal in soil human body and result is used for risk assessment.
Property method of testing can be given by the human body applied of commercialization as a kind of, while guaranteeing test result reliability, also need to possess proving installation and operating process is simple, can carry out batch samples test and realize the advantages such as control automatically simultaneously.Although domestic existing relevant patent of invention, proving installation is relatively complicated.As the test macro in the multi path artificial analogue gastronintestinal system assessment soil pollutant to human body validity method of Zhu Yong official rank invention comprises many polydisperse subsystems such as logical argon gas, stirring, the online titration of soda acid, pH on-line monitoring, complex operation, is difficult to control each sample and is in identical test environment.In a kind of dust/soil of the invention such as Lu Gaosheng the extraction method of simulated gastric fluid of absorption of human body heavy metal tested only heavy metal in human gastric juice do not test to property its in intestinal juice to property, result is difficult to objectively respond the actual human body of heavy metal to property.
Therefore; in view of the defect of existing related invention; the present invention propose one relatively simple, be easy to operation; and can comparatively objectively in simulated soil the human body of heavy metal release behavior in human intestines and stomach's digestive system give the convertible integrated test set of property and method, test result can be used in the efficiency assessment of health risk assessment and the risk control measure based on protection health.
Summary of the invention
The object of the invention is to propose a kind of heavy metal in soil human body to property reliable test result, proving installation and simple to operate, that batch samples test can be carried out integrated test set and method, can test to property for heavy metal-polluted soil human body, for heavy metal pollution place health risk assessment provides more objective Human body package concentration.For realizing above target, technical solution of the present invention is to provide a kind of heavy metal of simulating human consumption's feature to the convertible proving installation of property and method.
The convertible proving installation of giving property of heavy metal of simulation human consumption feature, it is characterized in that including extraction chamber, centre bearing, the Teflon extraction flask with cover of 12 2L, 12 hole fixed panels, centre bearing and upset motor contact, upset motor support fixture, upset motor, battery main switch, rotating mode switch, upset timer, rotating speed display and adjusting apparatus, Temperature displaying and adjusting apparatus, temperature sensor, cooling fan, heated fan, supply socket, connect wire, centre bearing securing member, control device room, extraction chamber's upset gland bonnet, the detachable radiation panel in pulpit.
Further, extraction chamber and control device room are integrated in a table apparatus, and heated fan, cooling fan, 12 hole control panels, temperature sensor are all integrated in extraction chamber.
Further, Temperature displaying and adjusting apparatus, rotating speed show with adjusting apparatus, rotating mode switch, overturns timer, overturn motor, the equal integrated installation of battery main switch is in control device indoor.
Further, 12 hole control panels and centre bearing are integral type parts, ensure that the stability of plant running in test process.
Further, centre bearing is firmly connected with upset motor with upset motor contact by centre bearing, guarantees the upset high efficiency of motor and the stability of plant running.
Further, temperature sensor, heated fan, cooling fan, Temperature displaying are connected to form a Temperature displaying and automatic control system with adjusting apparatus by being connected wire; First, the temperature value of extraction chamber is converted to electric signal by temperature sensor in real time, and be passed to Temperature displaying and adjusting apparatus by connecting wire, Temperature displaying and adjusting apparatus are converted into temperature reading and show after receiving electric signal; Meanwhile, the reading 37 DEG C of this reading and setting also compares by Temperature displaying and adjusting apparatus, as temperature reading <37 DEG C, starts heated fan; As temperature reading >37 DEG C, start cooling fan.
Further, upset motor, rotating speed display pass through to be connected wire with adjusting apparatus, battery main switch, rotating mode switch with upset timer and are connected to form one and overturn electric machine control system, carry out showing to motor overturning pattern, flip-flop transition, rotating speed and control.
Further, the convertible gland bonnet in extraction chamber is movable gland bonnet, carries out in process, cover the convertible gland bonnet in extraction chamber and seal extraction chamber in test, prevents extracting indoor temperature and reduces; After test terminates, open the convertible gland bonnet in extraction chamber, conveniently from 12 hole fixed panels, take out Teflon extraction flask with cover carries out sample separation.
Further, the detachable radiation panel in pulpit has heat radiation seam, can promote that overturning the used heat produced in motor operation course is dispersed into atmospheric environment, has ensured that upset motor long-time continuous is run.
A kind of heavy metal human body of simulating human intestines and stomach's digestion characteristics provided by the invention gives property convertible method of testing, comprises the following steps:
Step one: gather pedotheque, air-dry rear grinding and cross 0.25mm sieve, the soil sample of collection cut size <0.25mm is as testing sample;
Step 2: configuration artificial simulation gastric juices and intestinal juice, wherein NaCl concentration 5504 mg/L, NaH in artificial simulation gastric juices
2pO4 concentration 533mg/L, KCl concentration 1649mg/L, CaCl
2concentration 799mg/L, NH
4cl concentration 612mg/L, concentration of glucose 1300mg/L; Glucuronic acid concentration 40mg/L, uric acid 170mg/L, aminoglucose hydrochloride 660mg/L, bovine serum albumin 1000mg/L, pepsin 1000mg/L, adjust pH to 1.0 ± 0.2 of artificial simulation gastric juices with HCl; NaCl concentration 24542 mg/L, NaHCO3 concentration 22784mg/L, KCl concentration 1882mg/L, CaCl in artificial simulation intestinal juice
2concentration 422mg/L, MgCl
2concentration 100mg/L, uric acid 700mg/L, bovine serum albumin 2800mg/L, pancreatin 3000mg/L, lipase 500mg/L, bile prime 6000mg/L, the pH of artificial simulation intestinal juice is adjusted to 6.3 ± 0.2 by employing NaOH or HCl, the simulated gastric fluid of configuration and intestinal juice lid lid is sealed and be placed in water-bath be heated to 37 DEG C;
Step 3: 20g soil sample and 450ml simulated gastric fluid are added successively in 2L Teflon extraction flask with cover, after lid, manual overturning vibration 1min, measures the pH of simulated gastric fluid in bottle, guarantees that its value is 1.0 ± 0.2, otherwise adds HCl or NaOH adjustment pH to 1.2; Repetition like this, guarantees that continuous 3 pH readings are 1.0 ± 0.2; Cover tightly bottle cap sealing afterwards and extraction flask be fixed in the extraction flask fixed panel in extraction chamber;
Step 4: the temperature arranging extraction chamber is 37 DEG C, upset motor speed 60 revs/min, flip-flop transition 1h, inverted pattern for rotating forward, open upset motor control switch and begin turning extraction;
Step 5: after continuous overturning extracts 1h, close down upset motor, make its quiescent setting 5min, open bottle cover after taking off extraction flask, whether the pH of test simulation gastric juice is 1.0 ± 0.2; If so, then draw 10ml supernatant with 10ml glass syringe and cross 0.45 μm of filter membrane, after collecting filtrate with 10ml glass sample bottle, test the content of heavy metal in supernatant with ICP-MS, as the giving property of human body of peptic digest stage heavy metal in soil; Otherwise sample cancels, test of resampling;
Step 6: add 10ml simulated gastric fluid and 1200ml simulated intestinal fluid in extraction flask successively, pH to 6.8 is adjusted with NaOH or HCl, cover tightly manual overturning vibration 1min after bottle cap, open the pH of simulated intestinal fluid in bottle cap test bottle, guarantee that its value is 6.3 ± 0.2, otherwise add HCl or NaOH and adjust pH to 6.3 ± 0.2, so repeat, guarantee that continuous 3 pH readings are 6.3 ± 0.2; Cover tightly bottle cap sealing afterwards and extraction flask be fixed in the extraction flask fixed panel in extraction chamber;
Step 7: the temperature arranging extraction chamber is 37 DEG C, upset motor speed 60 revs/min, flip-flop transition 4h, inverted pattern for rotating forward, open upset motor control switch and begin turning extraction;
Step 8: after continuous overturning extracts 4h, close down upset motor, make its quiescent setting 5min, open bottle cover after taking off extraction flask, whether the pH of test simulation intestinal juice is 6.3 ± 0.2; If pH is 6.3 ± 0.2, then draw 10ml supernatant with 10ml glass syringe and cross 0.45 μm of filter membrane, collect filtrate with 10ml glass sample bottle and after adding 2ml HNO3, test the content of heavy metal in supernatant with ICP-MS, as the giving property of human body of intestinal digestion stage heavy metal in soil; Otherwise sample cancels, test of resampling.
Compared with prior art, the invention has the advantages that proving installation is simple, by upset extraction element, heating system, temperature online display and regulator control system, overturn motor speed and to show and regulator control system is integrated in a table apparatus.Meanwhile, the method for testing in the present invention is adjustment System pH after simulated gastric fluid tentatively mixes with soil sample with soil sample and simulated intestinal fluid respectively, makes it be stabilized in 1.0 ± 0.2 and 6.3 ± 0.2 respectively.And, repeatedly test experiments shows, after adopting process in this way, the pH environmental energy that stomach extracts stage and intestines extraction stage whole leaching process is continual and steady 1.0 ± 0.2 and 6.3 ± 0.2 respectively, avoid the adjustment of system pH in upset vibration test process, therefore, do not need to arrange pH on-line monitoring and acid base titration system, simplify operating process, reduce the complicacy of system.The convertible integrated test set of heavy metal-polluted soil that simulation human intestines and stomach in the present invention digests feature adopts 1 upset motor to drive 12 extraction flasks to carry out upset vibration simultaneously, can guarantee that the vibration operating mode of each extraction flask is consistent, make sample tests have comparability.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the integrated test set structural representation that the present invention proposes.
Fig. 2 is the integrated test set vertical view that the present invention proposes.
Fig. 3 is the integrated test set front view that the present invention proposes.
Fig. 4 is the integrated test set left view that the present invention proposes.
Fig. 5 is the integrated test set right view that the present invention proposes.
Reference numeral: 1-extraction chamber, 2-centre bearing, 3-2L Teflon extraction flask with cover, 4-12 hole fixed panel, 5-centre bearing and upset motor contact, 6-overturns motor support fixture, 7-overturns motor, 8-battery main switch, 9-rotating mode switch, 10-overturns timer, the display of 11-rotating speed and adjusting apparatus, 12-Temperature displaying and adjusting apparatus, 13-temperature sensor, 14-cooling fan, 15-heated fan, 16-supply socket, 17-connects wire, 18-centre bearing securing member, 19-control device room, the convertible gland bonnet in 20-extraction chamber, the detachable radiation panel in 21-pulpit.
Embodiment
Be specifically described below in conjunction with accompanying drawing 1-5.
The convertible proving installation of giving property of heavy metal of this simulation human consumption feature, include extraction chamber 1, centre bearing 2, the Teflon extraction flask 3 with cover of 12 2L, 12 hole fixed panels 4, centre bearing and upset motor contact 5, upset motor support fixture 6, upset motor 7, battery main switch 8, rotating mode switch 9, upset timer 10, rotating speed display and adjusting apparatus 11, Temperature displaying and adjusting apparatus 12, temperature sensor 13, cooling fan 14, heated fan 15, supply socket 16, connect wire 17, centre bearing securing member 18, control device room 19, extraction chamber's upset gland bonnet 20, the detachable radiation panel 21 in pulpit.
Further, extraction chamber 1 and control device room 19 are integrated in a table apparatus, and heated fan 15, cooling fan 14,12 hole control panel 4, temperature sensor 13 are all integrated in extraction chamber 1.
Further, Temperature displaying and adjusting apparatus 12, rotating speed show with adjusting apparatus 11, rotating mode switch 9, overturns timer 10, overturn motor 7, the equal integrated installation of battery main switch 8 is in control device room 19.
Further, be integral type parts in 12 hole control panels 4 and centre bearing 2, ensure that the stability of plant running in test process.
Further, centre bearing 2 is firmly connected with upset motor 7 with upset motor contact 5 by centre bearing, guarantees the upset high efficiency of motor 7 and the stability of plant running.
Further, temperature sensor 13, heated fan 15, cooling fan 14, Temperature displaying are connected to form a Temperature displaying and automatic control system with adjusting apparatus 11 by being connected wire 17; First, the temperature value of extraction chamber is converted to electric signal by temperature sensor 13 in real time, and be passed to Temperature displaying and adjusting apparatus 11 by connecting wire 17, Temperature displaying and adjusting apparatus 11 are converted into temperature reading and show after receiving electric signal; Meanwhile, the reading 37 DEG C of this reading and setting also compares by Temperature displaying and adjusting apparatus 11, as temperature reading <37 DEG C, starts heated fan 15; As temperature reading >37 DEG C, start cooling fan 14.
Further, upset motor 7, rotating speed display and adjusting apparatus 11, battery main switch 8, rotating mode switch 9 and upset timer 10 pass through to be connected wire 17 and are connected to form one and overturn electric machine control system, carry out showing to motor overturning pattern, flip-flop transition, rotating speed and control.
Further, the convertible gland bonnet 20 in extraction chamber is movable gland bonnets, carries out in process, cover convertible gland bonnet 20 pairs of extraction chambers 1 of extraction chamber and seal in test, prevents temperature in extraction chamber 1 from reducing; After test terminates, open the convertible gland bonnet 20 in extraction chamber, conveniently from 12 hole fixed panels 4, take out Teflon extraction flask 3 with cover carries out sample separation.
Further, the detachable radiation panel in pulpit (21) has heat radiation seam, can promote that overturning the used heat produced in motor (7) operational process is dispersed into atmospheric environment, has ensured that upset motor (7) long-time continuous is run.
Concrete method of testing step of the present invention is as follows:
(1) sample collection and pre-service
From heavy metal pollution place, gather 3 polluted soil sample by the representativeness that As, Cd, Pb pollute, cross 0.25mm sieve after natural air drying, the sample of collection cut size≤0.25mm is as test sample.
(2) configuration of artificial simulation gastric juices and intestinal juice
Artificial simulation gastric juices: get 1350ml deionized water, adds NaCl 7430.4mg, NaH successively
2pO
4719.55mg, KCl 2226.15mg, CaCl
21078.65mg, NH
4cl 826.2mg/L, glucose 1755mg; Glucuronic acid 54mg, uric acid 229.5mg, aminoglucose hydrochloride 891mg, bovine serum albumin 1350mg, pepsin 1350mg, with salt acid for adjusting pH to 1.0 ± 0.2;
Artificial simulation intestinal juice: get 3600ml deionized water, adds NaCl 883512mg, NaHCO successively
3820224mg, KCl 6775.2mg, CaCl
2151.2mg, MgCl
2360mg/L, uric acid 2520mg, bovine serum albumin 10080mg, pancreatin 10800mg, lipase 1800mg, bile prime 21600mg, adopt NaOH or HCl that the pH of artificial simulation intestinal juice is adjusted to 6.3 ± 0.2;
Before test experiments starts, the artificial simulation gastric juices configured and intestinal juice are positioned in water-bath and are heated to 37 DEG C.
(3) peptic digest stage heavy metal human body is tested to property
3 2L Teflon extraction flasks 3 put into by the sample getting 20g particle diameter≤0.25mm respectively, add the artificial simulation gastric juices that 450ml configures respectively, after covering bottle cap in manual overturning vibration 1min after in test bottle system pH and be adjusted to 1.0 ± 0.2 with HCl.Be fixed on after lid sealing is carried out to extraction flask in 12 hole fixed panels 4 in extraction chamber 1, cover the convertible gland bonnet 20 in extraction chamber.
Open the total power switch 8 of integrated test set, arrange upset motor speed be 55 turns/min, extract that indoor temperature is 37 DEG C, extraction time is 1h, inverted pattern for after rotating forward, start upset motor 7 and extract continuously.
After reaching setting extraction time, upset motor 7 stops automatically.Open the convertible gland bonnet 20 in extraction chamber, after taking out the static 5min of extraction flask, in test bottle, the pH of simulated gastric fluid is respectively 1.05,1.02,1.12, is all in 1.0 ± 0.2 scopes.Drawing after 0.45 μm of filter membrane crossed by 10ml supernatant with clean 10ml glass syringe is respectively collected in sample bottle, with ICP-MS test As, Cd, Pb concentration in supernatant as the peptic digest stage to property.
(4) intestinal digestion stage heavy metal human body is tested to property
First, supplement respectively in the extraction flask 3 in 10ml simulated gastric fluid to 3 step (3).Afterwards, add 1200ml simulated intestinal fluid respectively, after covering bottle cap after manual overturning vibration 1min in test bottle system pH and be adjusted to 6.3 ± 0.2 with NaOH or HCl.Be fixed in the 12 hole fixed panels 4 of in extraction chamber 1 after the sealing of lid lid is carried out to extraction flask, cover the convertible gland bonnet 20 in extraction chamber.
Open the total power switch 8 of integrated test set, arrange that upset motor speed is 55 turns/min, temperature is 37 DEG C in extraction chamber 1, extraction time is 4h, inverted pattern for after rotating forward, start upset motor 7 and extract continuously.
After reaching setting extraction time, upset motor 7 stops automatically.Open extraction chamber's gland bonnet, after taking out the static 5min of extraction flask, in test bottle, the pH of simulated gastric fluid is respectively 6.25,6.41,6.38, is all in 6.3 ± 0.2 scopes.Drawing after 0.45 μm of filter membrane crossed by 10ml supernatant with clean 10ml glass syringe is respectively collected in sample bottle, adds 1ml HNO
3, with ICP-MS test As, Cd, Pb concentration in supernatant as the intestinal digestion stage to property.
(5) in three soil sample samples of embodiment, the stomach of As, Cd, Pb, the human body in intestines stage give property test result respectively as shown in Table 1 and Table 2.
Claims (8)
1. a heavy metal of simulating human consumption's feature is to the convertible proving installation of property, it is characterized in that including extraction chamber (1), centre bearing (2), the Teflon extraction flask with cover (3) of 12 2L, 12 hole fixed panels (4), centre bearing and upset motor contact (5), upset motor support fixture (6), upset motor (7), battery main switch (8), rotating mode switch (9), upset timer (10), rotating speed display and adjusting apparatus (11), Temperature displaying and adjusting apparatus (12), temperature sensor (13), cooling fan (14), heated fan (15), supply socket (16), connect wire (17), centre bearing securing member (18), control device room (19), extraction chamber's upset gland bonnet (20), the detachable radiation panel in pulpit (21),
Extraction chamber (1) and control device room (19) are integrated in a table apparatus, and heated fan (15), cooling fan (14), 12 hole control panels (4), temperature sensor (13) are all integrated in extraction chamber (1);
Temperature sensor (13), heated fan (15), cooling fan (14), Temperature displaying are connected to form a Temperature displaying and automatic control system with adjusting apparatus (11) by being connected wire (17); First, the temperature value of extraction chamber is converted to electric signal by temperature sensor (13) in real time, be passed to Temperature displaying and adjusting apparatus (11) by connecting wire (17), Temperature displaying and adjusting apparatus (11) are converted into temperature reading and show after receiving electric signal; Meanwhile, the reading 37 DEG C of this reading and setting also compares by Temperature displaying and adjusting apparatus (11), as temperature reading <37 DEG C, starts heated fan (15); As temperature reading >37 DEG C, start cooling fan (14).
2. the heavy metal of simulation human consumption feature according to claim 1 gives property convertible proving installation, it is characterized in that Temperature displaying and adjusting apparatus (12), rotating speed show and adjusting apparatus (11), rotating mode switch (9), overturn timer (10), overturn motor (7), the equal integrated installation of battery main switch (8) is in control device room (19).
3. the convertible proving installation of giving property of heavy metal of simulation human consumption feature according to claim 1, is characterized in that 12 hole control panels (4) and centre bearing (2) are integral type parts, ensure that the stability of plant running in test process.
4. the convertible proving installation of giving property of heavy metal of simulation human consumption feature according to claim 1, it is characterized in that centre bearing (2) is firmly connected with upset motor (7) with upset motor contact (5) by centre bearing, guarantee to overturn the high efficiency of motor (7) and the stability of plant running.
5. the convertible proving installation of giving property of heavy metal of simulation human consumption feature according to claim 1, it is characterized in that upset motor (7), rotating speed display passes through to be connected wire (17) with adjusting apparatus (11), battery main switch (8), rotating mode switch (9) with upset timer (10) and be connected to form one and overturn electric machine control system, motor overturning pattern, flip-flop transition, rotating speed are carried out showing and controlled.
6. the convertible proving installation of giving property of heavy metal of simulation human consumption feature according to claim 1, it is characterized in that the convertible gland bonnet in extraction chamber (20) is movable gland bonnet, carry out in process in test, cover the convertible gland bonnet in extraction chamber (20) to seal extraction chamber (1), prevent the interior temperature in extraction chamber (1) from reducing; After test terminates, open the convertible gland bonnet in extraction chamber (20), convenient Teflon extraction flask with cover (3) that takes out from 12 hole fixed panels (4) carries out sample separation.
7. the convertible proving installation of giving property of heavy metal of simulation human consumption feature according to claim 1, it is characterized in that the detachable radiation panel in pulpit (21) having heat radiation seam, can promote that overturning the used heat produced in motor (7) operational process is dispersed into atmospheric environment, has ensured that upset motor (7) long-time continuous is run.
8. simulate the heavy metal of human consumption's feature to the convertible method of testing of property, its step comprises:
Step one: gather pedotheque, air-dry rear grinding and cross 0.25mm sieve, the soil sample of collection cut size <0.25mm is as testing sample;
Step 2: configuration artificial simulation gastric juices and intestinal juice, wherein NaCl concentration 5504 mg/L, NaH in artificial simulation gastric juices
2pO
4concentration 533mg/L, KCl concentration 1649mg/L, CaCl
2concentration 799mg/L, NH
4cl concentration 612mg/L, concentration of glucose 1300mg/L; Glucuronic acid concentration 40mg/L, uric acid 170mg/L, aminoglucose hydrochloride 660mg/L, bovine serum albumin 1000mg/L, pepsin 1000mg/L, adjust pH to 1.0 ± 0.2 of artificial simulation gastric juices with HCl; NaCl concentration 24542 mg/L, NaHCO in artificial simulation intestinal juice
3concentration 22784mg/L, KCl concentration 1882mg/L, CaCl
2concentration 422mg/L, MgCl
2concentration 100mg/L, uric acid 700mg/L, bovine serum albumin 2800mg/L, pancreatin 3000mg/L, lipase 500mg/L, bile prime 6000mg/L, the pH of artificial simulation intestinal juice is adjusted to 6.3 ± 0.2 by employing NaOH or HCl, the simulated gastric fluid of configuration and intestinal juice lid lid is sealed and be placed in water-bath be heated to 37 DEG C;
Step 3: 20g soil sample and 450ml simulated gastric fluid are added successively in 2L Teflon extraction flask with cover, after lid, manual overturning vibration 1min, measures the pH of simulated gastric fluid in bottle, guarantees that its value is 1.0 ± 0.2, otherwise adds HCl or NaOH adjustment pH to 1.2; Repetition like this, guarantees that continuous 3 pH readings are 1.0 ± 0.2; Cover tightly bottle cap sealing afterwards and extraction flask be fixed in the extraction flask fixed panel in extraction chamber;
Step 4: the temperature arranging extraction chamber is 37 DEG C, upset motor speed 60 revs/min, flip-flop transition 1h, inverted pattern for rotating forward, open upset motor control switch and begin turning extraction;
Step 5: after continuous overturning extracts 1h, close down upset motor, make its quiescent setting 5min, open bottle cover after taking off extraction flask, whether the pH of test simulation gastric juice is 1.0 ± 0.2; If so, then draw 10ml supernatant with 10ml glass syringe and cross 0.45 μm of filter membrane, after collecting filtrate with 10ml glass sample bottle, test the content of heavy metal in supernatant with ICP-MS, as the giving property of human body of peptic digest stage heavy metal in soil; Otherwise sample cancels, test of resampling;
Step 6: add 10ml simulated gastric fluid and 1200ml simulated intestinal fluid in extraction flask successively, pH to 6.8 is adjusted with NaOH or HCl, cover tightly manual overturning vibration 1min after bottle cap, open the pH of simulated intestinal fluid in bottle cap test bottle, guarantee that its value is 6.3 ± 0.2, otherwise add HCl or NaOH and adjust pH to 6.3 ± 0.2, so repeat, guarantee that continuous 3 pH readings are 6.3 ± 0.2; Cover tightly bottle cap sealing afterwards and extraction flask be fixed in the extraction flask fixed panel in extraction chamber;
Step 7: the temperature arranging extraction chamber is 37 DEG C, upset motor speed 60 revs/min, flip-flop transition 4h, inverted pattern for rotating forward, open upset motor control switch and begin turning extraction;
Step 8: after continuous overturning extracts 4h, close down upset motor, make its quiescent setting 5min, open bottle cover after taking off extraction flask, whether the pH of test simulation intestinal juice is 6.3 ± 0.2; If pH is 6.3 ± 0.2, then draws 10ml supernatant with 10ml glass syringe and cross 0.45 μm of filter membrane, collect filtrate with 10ml glass sample bottle and add 2ml HNO
3the content of heavy metal in supernatant is tested afterwards, as the giving property of human body of intestinal digestion stage heavy metal in soil with ICP-MS; Otherwise sample cancels, test of resampling.
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CN109975524A (en) * | 2019-05-08 | 2019-07-05 | 江苏省环境科学研究院 | It is a kind of simulation human stomach digest feature heavy metal biological can give system safety testing device and method |
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