WO2015074181A1 - 一种氮吹仪以及一种使用氮吹仪的湿法消解法 - Google Patents

一种氮吹仪以及一种使用氮吹仪的湿法消解法 Download PDF

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Publication number
WO2015074181A1
WO2015074181A1 PCT/CN2013/087431 CN2013087431W WO2015074181A1 WO 2015074181 A1 WO2015074181 A1 WO 2015074181A1 CN 2013087431 W CN2013087431 W CN 2013087431W WO 2015074181 A1 WO2015074181 A1 WO 2015074181A1
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Prior art keywords
digestion
nitrogen
cup
blowing
needle
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PCT/CN2013/087431
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English (en)
French (fr)
Inventor
李绍波
万渝平
梁恒兴
叶梅
张敏
乔秀明
陈代伟
曾琳
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成都市产品质量监督检验院
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Priority to PCT/CN2013/087431 priority Critical patent/WO2015074181A1/zh
Publication of WO2015074181A1 publication Critical patent/WO2015074181A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents

Definitions

  • the present invention relates to the field of experimental equipment, and more particularly to a nitrogen gas blower and a wet digestion method using a nitrogen gas blower.
  • wet digestion also known as wet ashing or wet oxidation, adding oxidizing strong acid to an appropriate amount of food, and simultaneously heating and decomposing, decomposing and decomposing organic substances into co 2 , water and various gases for accelerated oxidation
  • Various catalysts can be added at the same time.
  • This method of destroying organic substances in food is called wet digestion.
  • Biological samples containing a large amount of organic matter are usually wet-digested with a mixed acid, and the mixed acid used for wet digestion includes HN0 3 -HC104, HNO3-HCIO3-HCIO4, HNO3-HCIO4-H2SO4,
  • Nitric acid with a boiling point above 120 °C is a widely used pre-oxidant, which can destroy the organic matter in the sample; sulfuric acid has strong dehydration ability, can carbonize organic matter, partially degrade the insoluble matter and increase the boiling point of the mixed acid; Perchloric acid is the strongest oxidizing agent and dehydrating agent. Due to its high boiling point, it can continue to oxidize the sample after removing the nitric acid.
  • the oxidation of hydrogen peroxide in a mixed acid containing sulfuric acid is based on the formation of peroxymonosulfuric acid, which rapidly decomposes organic substances due to the dehydration of sulfuric acid.
  • the sample matrix contains more inorganic substances, it is mostly digested with a mixed acid containing hydrochloric acid; while hydrofluoric acid is mainly used to decompose the silicate-containing sample wet digestion is the most direct and effective for elemental analysis.
  • the most economical sample preparation method usually used for the detection of trace metal elements in food.
  • the existing wet digestion method generally involves placing a sample and a mixed acid into a digestion cup, and then placing the digestion cup on the heating device.
  • the mixed acid in the digestion process, the mixed acid generates a mixed acid vapor at a high temperature, and the acid in the digestion cup is gradually reduced.
  • the organic matter will produce black charcoal, and the charcoal will react with the nitric acid vapor and the perchloric acid vapor under the oxygen condition to burn, resulting in an explosion accident and a safety hazard.
  • Nitrogen blowing instrument is a device that purifies a heated liquid sample with nitrogen to rapidly concentrate the sample to be processed, and achieves rapid separation and purification. It is widely used in health, agriculture and environmental monitoring.
  • the needle and tubing materials of conventional nitrogen blowers are metal structures and are typically used for sample pretreatment of organic solvent extraction target components and cannot be used to treat strong acids or other corrosive solvents.
  • the present invention provides a new nitrogen blowing instrument, and provides a method for wet digestion using the nitrogen blowing instrument.
  • the nitrogen blowing instrument of the invention has a simple structure and can effectively prevent the detection environment.
  • the medium background value interferes with the target detection component and does not pollute the sample.
  • the wet digestion method of the invention can effectively solve the problem that the wet digestion in the prior art is prone to explosion, the operation risk is high, and the secondary pollution is caused. It is also possible to add a digestion solution at any time according to the digestion conditions to make the digestion more thorough.
  • the technical solution of the present invention is a nitrogen blowing instrument, comprising a bracket, a casing with a pipeline, a blowing needle and a heating device, and an upper part of the bracket is fixed with a casing placed with a pipeline, and a heating device is arranged at a lower portion of the bracket, and a pipeline is placed
  • the lower surface of the outer casing is provided with a detachable blowing needle, and the blowing needle is connected with the pipeline, and the pipeline and the blowing material are PTFE and a copolymer thereof.
  • the blowing needles are arranged in a matrix, five in the horizontal direction, four in the longitudinal direction, and the horizontal and vertical arrangement intervals are all 10 cm.
  • the heating device is an adjustable constant temperature heating device.
  • the heating device comprises a hot plate, the electric plate is 50 cm long and 40 cm wide.
  • the nitrogen blowing device further includes an infrared laser monitoring device, a liquid adding device, the infrared laser monitoring device is disposed on the lower bracket heating device, and the liquid adding device is disposed on the upper casing of the bracket.
  • the invention further provides a
  • the wet digestion apparatus includes a nitrogen gas blower and a digestion cup, and the digestion cup is placed on the nitrogen gas blower heating device.
  • the inner diameter of the blowing needle is 0. 5mnTl. 0mm, preferably 0.75mm, and the inner diameter of the digestion cup is 2cm ⁇ 6cm, preferably 4cm.
  • the invention also provides a wet digestion method using a nitrogen gas blower, characterized in that it comprises the steps of:
  • the total amount of the sample and the reaction reagent in the step 1) does not exceed one-fifth of the body of the digestion cup.
  • the length of the nitrogen blowing instrument in the step 3) extending into the digestion cup does not exceed two-fifths of the cup of the digestion cup.
  • the MPa is preferably 0. 15MPa.
  • the pressure is 0. lMPa ⁇ 0. 2MPa, preferably 0. 15MPa.
  • the digestion cup is digested with hydrofluoric acid when white crystals appear.
  • the beneficial effects of the invention are as follows:
  • the nitrogen atomizer of the invention has a simple structure, can effectively prevent the background value in the detection environment from interfering with the target detection component, and can not pollute the sample.
  • the wet digestion method of the invention has simple operation, effectively avoids the occurrence of explosion, improves the safety of operation, and is effective
  • the secondary pollution of the metal is avoided. It will not cause corrosion, clogging or dissolution of the needle and the pipeline, and will not pollute the sample. It is also possible to add a digestion solution at any time according to the digestion conditions to make the digestion more thorough.
  • Figure 1 is a schematic view showing the structure of a nitrogen blowing apparatus of the present invention
  • Figure 2 is a schematic view showing the nitrogen structure of the 7 liquid adding device of Figure 1 of the present invention.
  • Figure 3 is a flow chart of the method of using the nitrogen blowing instrument of the present invention.
  • the lower part of the bracket 1 is fixed with a heating device 6, and the lower surface of the outer casing 2 on which the pipeline is placed is provided with a detachable blowing needle 3, and the blowing needle 3 is connected with the pipeline, and the material of the pipeline and the blowing needle 3 is PTFE and Its copolymer.
  • the blowing needle is made of PTFE and its copolymer, which is not susceptible to corrosion and will not contaminate the sample when used for wet digestion.
  • the blow pins 3 are arranged in a matrix, five in the horizontal direction, four in the longitudinal direction, and the horizontal and vertical arrangement intervals are both 10 cm. The arrangement spacing is more suitable for digesting the size of the cup 4, so that the space of the nitrogen blowing instrument can be better utilized, the gas is not discharged poorly, and the conditions are gathered together to further ensure the safety of the operation.
  • the heating device 6 is an adjustable constant temperature heating device.
  • the heating device 6 includes a hot plate having a length of 50 cm and a width of 40 cm.
  • the nitrogen blowing device further includes an infrared laser monitoring device 8 and a liquid adding device 7.
  • the infrared laser monitoring device 8 is disposed on the lower heating device 6 of the bracket 1, and the liquid adding device 7 is disposed beside the upper casing of the bracket 1.
  • the infrared laser monitoring device 8 includes an infrared receiver and an infrared laser emission point.
  • the liquid in the digestion cup 4 is less than 15 mL
  • the liquid level in the digestion cup 4 is detected by an infrared laser at 905 nm and an infrared receiver. 7 ⁇
  • the height of the receiving point of the infrared receiver is adjusted to 1. 7cm.
  • the intensity of the infrared laser received by the infrared light receiver changes, thereby exciting the liquid adding device 7, the liquid adding device 7 including the controller, the liquid storage container and the tube road.
  • the liquid adding device 7 can adjust the filling volume, and the filling volume is adjustable from 1 mL to 20 mL in 20 steps; the liquid adding device 7 has four liquid storage containers 9 respectively placed with different solutions, and respectively added to the mixed liquid container through the adding liquid line 11 12 in.
  • a valve 10 is provided on the liquid supply line 1 1 .
  • the solution in the mixed liquid container 12 is added to the digestion cup 4 through the mixed liquid line 14.
  • a valve two 13 is disposed on the mixed liquid line 14.
  • Valve one 10 and valve two 13 are electric valves.
  • the controller controls the opening and closing of the valve 10 and the valve 2 on the liquid supply line 11 and the mixed liquid line 14 by the signal of the infrared laser monitoring device 8 and a preset program to achieve the purpose of adding liquid.
  • the liquid addition device 7 may be added not only to the solution but also to the digestion vessel 4 after mixing the solution in the mixing container 12.
  • a digestion cup 4 can be provided with a liquid addition device 7, and a liquid addition device 7 can also be used to add liquid to a plurality of digestion cups 4. This design not only compensates for the judgment error of the experimental operator in the digestion process. It also frees the experimental operator from dangerous and heavy work. Of course, the experimental operator can also observe the amount of the digestion liquid by the naked eye, manually configure the mixed acid, and manually set the filling volume.
  • the present invention also provides a wet digestion method using a nitrogen gas blower. Weigh 0. 5 ⁇ 5g sample, the sample amount can be adjusted according to the sample density, fat content and the content of the metal element to be tested. Place the weighed sample in the digestion cup 4, and add 1 (T20mL nitric acid and perchloric acid mixed reagent, the volume ratio of nitric acid to perchloric acid is 5: 1.
  • the total amount of sample and reaction mixture 5 No more than one-fifth of the cup of the digestion cup.
  • the diameter of the digestion cup 4 is 2cnT6c m , preferably 4cm.
  • the inner diameter of the digestion cup is less than 2cm, the digestion solution cannot be sufficiently contacted with the sample to be digested, thereby The digestion efficiency is reduced; within the allowable nitrogen flow range, when the diameter of the digestion cup is greater than 6 cm, the nitrogen cannot fill the entire digestion cup, so that the digestion solution in the digestion cup is not sufficiently insulated from the environmental pollutants.
  • the apparatus 6 is adjusted to 100 ° C, the digestion cup 4 is placed on the heating device 6, the nitrogen blowing instrument needle 3 is placed in the digestion cup 4, and the nitrogen blowing instrument needle 3 is extended into the digestion cup 4 and the length does not exceed the digestion cup. 4 1/2 cup body.
  • the inner diameter of the needle is 0. 5mnTl. O ⁇ , preferably 0. 75 ⁇ , the experiment proves that when the inner diameter of the needle is less than 0. 5mm, if the appropriate nitrogen flow rate is to be achieved, it must be added Large nitrogen pressure, after nitrogen pressure is increased The pressure on the nitrogen flow path is extremely high, and the life of the nitrogen flow path is shortened. When the inner diameter of the needle is greater than 1.0 mm, the nitrogen will be scattered, and the nitrogen can not be effectively filled with the entire digestion cup.
  • the digestion liquid is always in a boiling state, if the nitrogen blowing instrument is inserted into the needle 3
  • the length of the digestion cup 4 exceeds the two-fifth cup of the digestion cup 4
  • the digestion liquid adheres to the blow needle 3 and causes the digestion liquid to splash out of the digestion cup 4, thereby causing the measurement result to be low.
  • the liquid is the sample and the reaction reagent mixture. Pass the protective gas, and after the reddish brown smoke disappears, slowly increase the temperature of the heating device 6 to 160 ° C until the sample is clear and transparent.
  • the temperature of the heating device 6 is raised to 200 ° C and heating is continued until the sample solution is lower than 5 mL. 20 mL of ultrapure water is added to the heating device 6 at 100 ° C to catch the acid. Until the solution below 5mL, digestion removed the cup 4, And set to room temperature. Transfer with ultrapure water and dilute to 25mL, and check on the machine.
  • the shielding gas is typically nitrogen. 2MPa ⁇ 0MPa ⁇ The pressure is 0. lMPa ⁇ 0. 2MPa. If the purity of the nitrogen is less than 99.2%, there is a risk that impurities in the cylinder will be carried into the digestion cup 4. If the nitrogen pressure is lower than 0.
  • the gas flow is small, and it is not possible to prevent the liquid droplets suspended from the outside from entering the digestion cup 4. If the nitrogen pressure is higher than 0.2 MPa, the gas flow is large, which will cause the digestion liquid in the digestion cup 4 to be sprayed outside the digestion cup 4, resulting in a low measurement result, and also causes the digestion liquid to evaporate too quickly. Increase the amount of digestion solution and the background interference of the digestion solution.
  • the protective gas is introduced through a nitrogen gas blowing device, and the nitric acid vapor, the perchloric acid vapor, the oxygen gas, and the like in the digestion cup 4 are discharged into the digestion cup 4 during the digestion, so that the nitric acid vapor, the perchloric acid vapor, and the oxygen are not in contact with the carbonized material, so that The mixing concentration between each other is lowered, and the probability of explosion is greatly reduced.
  • the shielding gas fills the digestion cup 4, so that the acid vapor mixed with the metal element does not have a chance to flow back into the digestion cup 4. Avoid secondary pollution of metals.
  • the experiment proves that when the volume of the digestion cup is 60mL, the inner diameter is 4cm, the inner diameter of the needle is 0. 75mm, the protective gas pressure is 0. 15MPa, the digestion effect is the best, and the safest in the digestion process, the metal of the inspection
  • the secondary pollution is the least, and it will not cause corrosion, clogging or dissolution of the needle and the pipeline, and will not pollute the sample.
  • the oil content is more than 30%, it is a sample with high oil content; when it is digested to the sample without brown or yellow smoke, if there is visible crystal on the bottom of the digestion cup, it is high in inorganic content.
  • the inventors generally adjust the temperature, time, and digesting solution dosage according to the nature of the sample. When digesting samples with high oil content, it is possible to increase the time of pre-digestion and reduce the proportion of perchloric acid in the mixed acid, even without adding perchloric acid. In the digestion of samples with high inorganic content, the inventors will increase the temperature, increase the digestion time and add other acids to help improve the digestion.
  • fern root powder as a common food
  • some white crystals cannot be completely eliminated when using conventional digestion methods.
  • the temperature is generally increased by 50 °C on the basis of the original, and the digestion time is prolonged. 6 (T90min, and adding hydrofluoric acid to the white crystal in the digestion cup to improve the digestion effect, and finally let the white crystal dissolve completely.

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Abstract

一种氮吹仪，包括支架（1）、放置有管路的外壳（2）、吹针（3）和加热装置（6）。支架（1）上部固定有放置有管路的外壳（2），支架（1）下部固定有加热装置（6），放置有管路的外壳（2）下表面设置有可拆卸的吹针（3），吹针（3）与管路相连。管路与吹针材料为聚四氟乙烯及其共聚物。一种使用该氮吹仪的湿法消解法，包括步骤：1）将试样和反应试剂放置到消解杯内；2）将消解杯放置到氮吹仪加热装置上；3）将氮吹仪吹针放入消解杯中，通入保护气体；4）根据试样和反应试剂的种类，按照预设的消解温度设定或改变加热装置的加热温度。该氮吹仪结构简单，用于湿法消解可以有效地避免爆炸，提高操作的安全性，还可以有效地避免金属的二次污染，保证检测结果的准确度。

Description

一种氮吹仪以及一种使用氮吹仪的湿法消解法 技术领域
本发明涉及实验设备技术领域， 尤其涉及一种氮吹仪以及一种使用氮吹 仪的湿法消解法。
背景技术
湿法消解，又称湿灰化法或湿氧化法，在适量的食品中加入氧化性强酸， 并同时加热消煮， 使有机物质分解氧化成 co2， 水和各种气体， 为加速氧化 进行， 可同时加入各种催化剂， 这种破坏食品中有机物质的方法就叫做湿法 消解。 含有大量有机物的生物样品通常采用混酸进行湿法消解， 用于湿法消 解的混酸包括 HN03-HC104 、 HNO3-HCIO3-HCIO4、 HNO3-HCIO4-H2SO4、
HN03_H2S04、 H2S04-H202和 HN03-H202。 其中沸点在 120°C以上的硝酸是广泛 使用的预氧化剂， 它可破坏样品中的有机质； 硫酸具有强脱水能力， 可使有 机物炭化， 使难溶物质部分降解并提高混合酸的沸点； 热的高氯酸是最强的 氧化剂和脱水剂， 由于其沸点较高， 可在除去硝酸以后继续氧化样品。 在含 有硫酸的混合酸中过氧化氢的氧化作用是基于过一硫酸的形成， 由于硫酸的 脱水作用， 该混合溶液可迅速分解有机物质。 当样品基体含有较多的无机物 时， 多采用含盐酸的混合酸进行消解； 而氢氟酸主要用于分解含硅酸盐的样 口 湿法消解是目前做元素分析的最直接、 最有效、 最经济的一种样品前处 理手段， 通常用于食品的痕量金属元素检测。 现有的湿法消解法一般是将试样与混酸置入消解杯中， 再将消解杯放到 加热装置上。 现有的湿法消解方法， 在消解过程中， 混合酸在高温下会生成 混酸蒸汽， 消解杯中的酸会慢慢减少。 随着酸的减少， 有机物会产生黑色炭 化物， 而炭化物在氧气条件下会与硝酸蒸汽、 高氯酸蒸汽发生反应而燃烧， 导致爆炸事故， 存在安全隐患。
氮吹仪是一种采用氮气对加热液体样品进行吹扫， 使待处理样品迅速浓 缩， 达到快速分离纯化效果的装置， 广泛应用于卫生、 农业及环境监测等领 域。 传统氮吹仪的吹针和管路材料都是金属结构， 通常用于有机溶剂提取目 标检测组分的样品前处理， 不能用于处理强酸或者其他腐蚀性溶剂。
发明内容
为了解决现有湿法消解的问题， 本发明提供了一种新的氮吹仪， 同时提 供了使用该氮吹仪进行湿法消解的方法，本发明氮吹仪结构简单，能有效防止 检测环境中背景值对目标检测组份的干扰， 且不会对样品造成污染。 本发明 湿法消解方法能有效解决现有技术中湿法消解易发生爆炸、 操作危险性大、 有二次污染的问题。 还能根据消解情况随时添加消解液， 让消解更彻底。
本发明的技术方案是一种氮吹仪， 包括支架、 放置有管路的外壳、 吹针 和加热装置， 支架上部固定有放置有管路的外壳，支架下部固定有加热装置， 放置有管路的外壳下表面设置有可拆卸的吹针， 吹针与管路相连， 管路与吹 针材料为聚四氟乙烯及其共聚物。
优选的， 所述吹针成矩阵排列， 横向排列 5根， 纵向排列 4根， 横向和 纵向的排列间距均为 10cm。
进一步的， 所述加热装置为可调恒温加热装置。
优选的， 所述加热装置包括电热板， 所述电热板长 50cm， 宽 40cm。 进一步的，所述氮吹仪还包括红外激光监测装置、加液装置，所述红外激 光监测装置设置在支架下部加热装置上， 所述加液装置设置在支架上部外壳 本发明还提供了一种湿法消解装置， 包括氮吹仪和消解杯， 所述消解杯 放置在氮吹仪加热装置上。
优选的， 所述吹针内径为 0. 5mnTl. 0mm， 优选为 0. 75mm， 所述消解杯的 内径为 2cm〜6cm， 优选为 4cm。
本发明还提供了一种使用氮吹仪的湿法消解法，其特征在于， 包括步骤:
1 ) 将试样和反应试剂放置到消解杯内；
2 ) 再将消解杯放置到氮吹仪加热装置上；
3 ) 将氮吹仪吹针放入消解杯中， 通入保护气体；
4)根据试样和反应试剂的种类，按照预设的消解温度设定或改变加热装 置的加热温度。
优选的， 所述步骤 1 ) 中的试样和反应试剂的总量不超过消解杯五分之 一杯身。
进一步的， 所述步骤 3 ) 中的氮吹仪吹针伸入消解杯内的长度不超过消 解杯五分之二杯身。
进一步的， 所述步骤 3 ) 中的保护气体是氮气， 所述氮气的纯度不低于 99. 2 % , 压力为 0. lMPa〜0. 2MPa， 优选的为 0. 15MPa。
优选的， 所述步骤 3 ) 中消解杯在出现白色晶体时， 加入氢氟酸消解。 本发明的有益效果是： 本发明氮吹仪其结构简单， 能有效防止检测环境 中背景值对目标检测组份的干扰， 且可不会对样品造成污染。 本发明湿法消 解方法操作简单， 有效的避免了爆炸的发生， 提高了操作的安全性， 还有效 的避免了金属的二次污染。且不会造成吹针和管路的腐蚀变形、堵塞或溶解， 不会对样品造成污染。 还能根据消解情况随时添加消解液， 让消解更彻底。 附图说明
图 1为本发明氮吹仪结构示意图；
图 2为本发明图 1中 7加液装置氮结构示意图；
图 3为本发明氮吹仪使用方法的流程图；
图中： 1.支架， 2.放置有管路的外壳， 3.吹针， 4.消解杯， 5.试样和反应试 剂混合物即消解液， 6.加热装置， 7.加液装置， 8.红外激光监测装置， 9.储 液容器， 10.阀门一， 11.加液管路， 12. 混液容器， 13.阀门二， 14.混液管 路。
具体实施方式
为了使本发明的目的、 技术方案及优点更加清楚明白， 以下结合附图， 对本发明进行进一步详细说明。
如图 1、 图 2所示， 本发明提供的一种氮吹仪， 包括支架 1、放置有管路 的外壳 2、 吹针 3和加热装置 6， 支架 1上部固定有放置有管路的外壳 2，支 架 1下部固定有加热装置 6，放置有管路的外壳 2下表面设置有可拆卸的吹针 3， 吹针 3与管路相连，管路与吹针 3材料为聚四氟乙烯及其共聚物。吹针采 用聚四氟乙烯及其共聚物， 不易受腐蚀， 用于湿法消解时， 不会污染试样。 吹针 3成矩阵排列， 横向排列 5根， 纵向排列 4根， 横向和纵向的排列间距 均为 10cm。这种排列间距更能适合消解杯 4的尺寸大小， 使其更好的利用氮 吹仪的空间， 不会造成气体排出不畅， 汇集一起等状况， 进一步保证了操作 的安全。 加热装置 6为可调恒温加热装置。 加热装置 6包括电热板， 电热板 长 50cm, 宽 40cm。 氮吹仪还包括红外激光监测装置 8、 加液装置 7， 红外激光监测装置 8 设置在支架 1下部加热装置 6上， 加液装置 7设置在支架 1上部外壳旁。 红 外激光监测装置 8包括红外接收器和红外激光发射点。 当消解杯 4内的液体 低于 15mL时，通过 905nm红外激光，和红外接收器来检测消解杯 4内液面高 度。 因为消解杯 4底厚 0. 5cm， 调整红外激光发射点， 和红外接收器接收点 的高度至 1. 7cm。 当消解杯 4内液面到杯底的距离小于 1. 2cm时， 红外光接 收器接收的红外激光强度发生变化， 从而激发加液装置 7， 加液装置 7包括 控制器、 储液容器和管路。 加液装置 7 可以调整加液体积， 加液体积从 lmL〜20mL分 20档可调； 加液装置 7有四个储液容器 9分别放置不同溶液， 分别通过加液管路 11加入到混液容器 12中。 加液管路 1 1上设置有阀门一 10。 混液容器 12中的溶液通过混液管路 14将溶液加入到消解杯 4中。 混液 管路 14上设置有阀门二 13。 阀门一 10与阀门二 13为电动阀门。 控制器通 过红外激光监测装置 8的信号与预设的程序控制加液管路 11与混液管路 14 上的阀门一 10和阀门二 13的开闭， 达到加液目的。 加液装置 7不但可以单 独加入溶液也可以将溶液在混液容器 12中混合后再加入到消解杯 4中。一个 消解杯 4可以配套一个加液装置 7， 一个加液装置 7也可以对应给多个消解 杯 4加液。 这个设计不仅弥补了实验操作人员在消解过程中， 对消解液余量 的判断误差。 也让实验操作人员从危险、 繁重的工作中解脱出来。 当然实验 操作人员也可以通过肉眼观察消解液余量， 手动配置混酸， 手动设置加液体 积。
发明人在做痕量金属元素的检测时发现消解杯 4外部夹杂着金属元素的 酸蒸汽回流到消解杯 4中， 造成痕量金属样品的二次污染， 所以痕量金属元 素的检测时， 会造成检测结果偏差较大。 如图 3 所示， 本发明还提供了一种使用氮吹仪的湿法消解法。 称取 0. 5〜5g试样，可根据样品密度、脂肪含量和待测金属元素的含量调整称样量。 将称取的试样置于消解杯 4中，加入 l(T20mL硝酸和高氯酸混合的反应试剂， 硝酸和高氯酸的体积比例为 5 : 1。 试样和反应试剂混合物 5的总量不超过消 解杯 4五分之一杯身。所述消解杯 4的直径为 2cnT6cm， 优选的为 4cm， 实验 证明，如果消解杯内径小于 2cm， 消解液不能够与待消解样品充分接触， 从而 使消解效率降低； 在允许的氮气流量范围内， 当消解杯直径大于 6cm时， 氮 气不能够充满整个消解杯， 从而使消解杯内消解样液与环境中的污染物不能 够充分隔绝。 把加热装置 6调至 100°C， 把消解杯 4置于加热装置 6上， 将 氮吹仪吹针 3放入消解杯 4内， 氮吹仪吹针 3伸入消解杯 4内长度不超过消 解杯 4五分之二杯身。 吹针内径为 0. 5mnTl . O匪， 优选的为 0. 75匪， 实验证 明，当吹针内径小于 0. 5mm时，如果要达到合适的氮气流量，必须加大氮气的 压力， 氮气压力加大后， 对氮气流路管道造成极大压力， 缩短了氮气流路管 道的寿命； 当吹针内径大于 1. 0mm时， 氮气会发生散流， 不能够有效的让氮 气充满整个消解杯， 此外， 当吹针内径大于 1. 0mm时， 要达到隔绝环境污染 物的效果， 势必增加氮气的消耗量， 增加实验成本。 在消解过程中， 消解液 始终处于沸腾状态的， 如果氮吹仪吹针 3伸入消解杯 4内长度超过消解杯 4 五分之二杯身时， 会有消解液粘附于吹针 3和造成消解液喷溅到消解杯 4外 的可能， 从而造成测定结果的偏低。 消解液为试样和反应试剂混合物。 通入 保护气体， 待红棕色烟雾消失后慢慢提高加热装置 6温度至 160°C， 直到试 样清亮透明。 消解过程中如果样液颜色变深， 滴加硝酸让颜色变转回来。 把 加热装置 6温度提高至 200°C继续加热， 直至试样溶液低于 5mL， 加入 20mL 超纯水置于 100°C加热装置 6上，赶酸，直至溶液低于 5mL时，取下消解杯 4， 并放置至室温。 用超纯水转移并定容至 25mL， 上机检测。 保护气体一般为氮 气。 氮气的纯度不低于 99. 2 % , 压力为 0. lMPa〜0. 2MPa。 如果氮气纯度低于 99. 2%, 可能会有把气瓶中的杂质带入消解杯 4 的风险。 如果氮气压力低于 0. IMPa, 气流较小， 不能够起到阻挡外界悬浮的酸液滴进入消解杯 4的现象 发生。 如果氮气压力高于 0. 2MPa， 由于气流量较大， 会造成消解杯 4中的消 解液喷溅到消解杯 4外， 造成测定结果的偏低， 此外也会造成消解液的挥发 过快，增加消解液的使用量和消解液的本底干扰。使用氮吹仪通入保护气体， 在消解中将消解杯 4中的硝酸蒸汽、 高氯酸蒸汽、 氧气等排出消解杯 4， 使 硝酸蒸汽、 高氯酸蒸汽、 氧气不与炭化物接触， 使其相互之间的混合浓度降 低， 使发生爆炸的几率大大降低。 且通入保护气体后， 保护气体充满了消解 杯 4， 使夹杂着金属元素的酸蒸汽没有机会回流到消解杯 4中。 避免了金属 的二次污染。
实验证明，当消解杯容积为 60mL、 内径为 4cm， 吹针内径为 0. 75mm， 保 护气体压强为 0. 15MPa时， 消解的效果最好， 且在消解过程中最安全， 检查 时金属的二次污染最少， 且不会造成吹针和管路的腐蚀变形、 堵塞或溶解， 不会对样品造成污染。
由于食品样品种类繁多， 有含油高的或含油低的， 有无机质含量高的或 含量低的。 含油量大于 30%时， 即为含油量高样品； 当消解至样液无棕色或 黄色烟雾时， 如果消解杯底部有肉眼可见晶体时， 即为无机质含量高。 发明 人一般会根据样品性质对温度、 时间、 消解液剂量进行调整。 在消解含油高 的样品时， 可以增加预消解的时间， 并且减少高氯酸在混酸中的比例， 甚至 可以不加高氯酸。 在消解无机质含量高的样品时， 发明人会提高温度、 增加 消解时间和加入其它酸来帮助改善消解效果。例如：蕨根粉作为常见的食品， 因为其无机质含量较高， 在采用常规消解方法时， 会有一些白色结晶不能够 消解完全， 为了达到满意的消解效果， 一般会把温度在原来的基础上提高 50 °C， 把消解时间延长 6(T90min， 并在消解杯中出现白色结晶时加入氢氟酸来 改善消解效果， 最终让白色结晶消解完全。
当然， 本发明还可有其它多种实施例， 在不背离本发明精神及其实质的 情况下， 熟悉本领域的技术人员可根据本发明作出各种相应的改变和变形， 但这些相应的改变和变形都应属于本发明所附的权利要求的保护范围。

Claims

权 利 要 求 书
1、 一种氮吹仪， 其特征在于： 包括支架、 放置有管路的外壳、 吹针和加 热装置，所述支架上部固定有放置有管路的外壳，所述支架下部固定有加热装 置，所述放置有管路的外壳下表面设置有可拆卸的吹针， 所述吹针与管路相 连， 所述管路与吹针材料为聚四氟乙烯及其共聚物。
2、 根据权利要求 1所述的氮吹仪， 其特征在于： 所述吹针成矩阵排列， 横向排列 5根， 纵向排列 4根， 横向和纵向的排列间距均为 10cm。
3、根据权利要求 1所述的氮吹仪， 其特征在于： 所述加热装置为可调恒 温加热装置。
4、根据权利要求 1所述的氮吹仪， 其特征在于： 所述加热装置包括电热 板， 所述电热板长 50cm， 宽 40cm。
5、根据权利要求 1所述的氮吹仪， 其特征在于： 还包括红外激光监测装 置、 加液装置， 所述红外激光监测装置设置在支架下部加热装置上， 所述加 液装置设置在支架上部外壳上。
6、一种湿法消解装置， 其特征在于： 包括权利要求 1-5所述的氮吹仪和 消解杯， 所述消解杯放置在氮吹仪加热装置上。
7、根据权利要求 6所述的湿法消解装置， 其特征在于： 所述吹针内径为 0. 5mm" 1. 0mm, 优选为 0. 75mm。
8、根据权利要求 6所述的湿法消解装置， 其特征在于： 所述消解杯的内 径为 2cm〜6cm， 优选为 4cm。
9、一种使用权利要求 1-5所述的氮吹仪的湿法消解法，其特征在于， 包 括步骤：
1 ) 将试样和反应试剂放置到消解杯内； 2 ) 再将消解杯放置到氮吹仪加热装置上；
3 ) 将氮吹仪吹针放入消解杯中， 通入保护气体；
4)根据试样和反应试剂的种类，按照预设的消解温度设定或改变加热装 置的加热温度。
10、 根据权利要求 9所述的氮吹仪使用方法， 其特征在于： 所述步骤 1 ) 中的试样和反应试剂的总量不超过消解杯五分之一杯身。
11、 根据权利要求 9所述的氮吹仪使用方法， 其特征在于： 所述步骤 3 ) 中的氮吹仪吹针伸入消解杯内的长度不超过消解杯五分之二杯身。
12、 根据权利要求 9所述的氮吹仪使用方法， 其特征在于： 所述步骤 3 ) 中的保护气体是氮气， 所述氮气的纯度不低于 99. 2 %。
13、 根据权利要求 9所述的氮吹仪使用方法， 其特征在于： 所述步骤 3 ) 中的保护气体是氮气， 所述氮气压力为 0. lMPa〜0. 2MPa， 优选为 0. 15MPa。
14、 根据权利要求 9所述的氮吹仪使用方法， 其特征在于： 所述步骤 3 ) 中， 消解杯内出现白色晶体时， 加入氢氟酸消解。
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