CN111239323A - Rapid detection method for hazardous waste hazard characteristics - Google Patents
Rapid detection method for hazardous waste hazard characteristics Download PDFInfo
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- CN111239323A CN111239323A CN202010089949.9A CN202010089949A CN111239323A CN 111239323 A CN111239323 A CN 111239323A CN 202010089949 A CN202010089949 A CN 202010089949A CN 111239323 A CN111239323 A CN 111239323A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/80—Indicating pH value
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/18—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react
Abstract
The invention provides a method for rapidly detecting hazardous characteristics of hazardous waste, which sequentially comprises the following steps: s1, mixing a sample with water, and observing whether a reaction occurs or not; s2, if no reaction exists, judging a soluble result; s3, dripping the sample solution onto pH test paper, and judging the pH value of the sample; s4, dripping the sample solution onto potassium iodide starch test paper, and judging an oxidation test result; s5, adding triethylamine, uniformly mixing, recording the temperature of the solution at the moment, and judging a polymerization result; s6, adding a hydrochloric acid solution, wetting lead acetate test paper, attaching the lead acetate test paper to the inner wall of the container, and judging a sulfide result; s7, adding a sulfuric acid solution for acidification, placing cyanide test paper on a container opening, immediately plugging the container opening by using a plug, and placing the container opening into a water bath at 70 ℃ to judge the result of cyanide in the sample; s8, putting the sample into an aluminum weighing boat, igniting a gas torch, and judging the flammability result. The method disclosed by the invention can be used for rapidly judging the hazard characteristics of the hazardous waste and reducing the reagent configuration.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for rapidly detecting hazardous characteristics of hazardous waste.
Background
The hazardous waste refers to solid waste which is listed in a national hazardous waste list or is determined according to the national hazardous waste identification standard and identification method, has one or more hazardous characteristics such as corrosivity, toxicity, flammability, reactivity and infectivity, and does not exclude the hazardous characteristics. The standard method needs to pass through more complicated steps in a laboratory, uses more reagents, consumes longer time, and needs to test through equipment, the hazardous characteristics of the hazardous waste often need to be analyzed quickly to judge the packaging, transportation and storage modes of the waste so as to achieve safe transportation and storage, and a detection method with quick and simple judgment is needed.
Disclosure of Invention
The method aims to rapidly judge the hazard characteristics of the hazardous waste, reduce reagent configuration, and rapidly judge the hazardous characteristics below the waste without large-scale detection equipment.
The technical scheme of the invention is realized as follows:
the invention provides a method for rapidly detecting hazardous characteristics of hazardous waste, which sequentially comprises the following steps:
s1, mixing a sample with water in a container, and observing whether a reaction occurs or not;
s2, if no reaction exists, recording the solubility as soluble, partially soluble and insoluble according to the solubility;
s3, dripping one or more drops of sample solution onto pH test paper, judging and recording the pH value of the solution, and judging the pH value of the sample;
s4, dripping one or a plurality of drops of sample solution on potassium iodide starch test paper, wherein if the test paper is blue, the oxidation test result is positive, otherwise, the oxidation test result is negative;
s5, adding triethylamine into a part of sample solution, uniformly mixing, immediately inserting a thermometer, recording the temperature of the solution at the moment, and if any one or more of temperature rise, air release, polymerization and gelation occur, judging that the polymerizability is positive, otherwise, judging that the polymerizability is negative;
s6, adding a hydrochloric acid solution into a part of sample solution, fully mixing, wetting lead acetate test paper, enabling the lead acetate test paper to be attached to the inner wall of the container and not to be in contact with the sample solution, if the lead acetate test paper is changed into silver brown or black, judging that the result of sulfide in the sample is positive, otherwise, judging that the result is negative;
s7, adding a sulfuric acid solution into a part of sample solution for acidification, slowly adjusting the mixed solution to be strongly acidic, placing a cyanide test paper on a container opening, enabling the bottom of the test paper to be above the liquid level, enabling the other part of the test paper to extend out of the container opening and not to be in contact with the sample solution, immediately plugging the container opening by using a plug, placing the container opening into a water bath at 70 ℃, if the middle of the test paper turns blue, judging that the result of the cyanide in the sample is positive, otherwise, judging that the result is negative;
s8, putting a sample into an aluminum weighing boat, igniting a gas torch, adjusting to a blue flame which is not easy to extinguish, wherein the flame of the gas torch does not contact the sample, judging that the sample has inflammability if an ignition phenomenon is observed, continuing to test if the sample is not ignited, putting the flame on the sample for at least 15 seconds, judging that the flammability test result is positive if the ignition phenomenon is observed, and judging that the flammability result is negative if the sample is decomposed, boiled or continuously heated by lamp flame for 15 seconds and is not ignited;
s9, result evaluation:
a) if the pH value is less than 4 or greater than 10, the pH value is determined to be acidic and corrosive;
b) is determined to be "water compatible" if not reactive with water;
c) if the oxidability test is positive, determining that the product has oxidability;
d) if the test of polymerizability is positive, determining that the polymer is 'polymerizability';
e) if the cyanide and sulfide test is positive, the cyanide and sulfide are determined to be "cyanide" and "sulfide";
f) if the flammability test is positive, then it is determined to be "flammable";
g) whether the waste sample is "dangerous" is finally determined according to the above description of the dangerous characteristics.
As a further improvement of the present invention, the mass-to-volume ratio or the volume ratio of the sample and the water in step S1 is 1: 10.
As a further improvement of the present invention, the method for observing whether to react in step S1 is to determine whether smoke, gas release, precipitation, creaminess and obvious temperature change occur, and if any one or more of the conditions occur, the reaction is determined, otherwise, the reaction is not determined.
As a further improvement of the present invention, the volume ratio of the triethylamine to the sample solution in step S5 is 1: (0.8-1.5).
As a further improvement of the invention, the preparation method of the hydrochloric acid solution in the step S6 is to mix concentrated hydrochloric acid and water uniformly according to the volume ratio of 1: 1.
As a further improvement of the present invention, the volume ratio of the hydrochloric acid solution to the sample solution in step S6 is 5: (3-5).
As a further improvement of the present invention, the strongly acidic pH in step S7 is 1-2.
As a further improvement of the present invention, the ignition phenomenon in step S8 includes a flash of light or burning.
As a further development of the invention, the container is a test tube, beaker or flask.
Water compatibility, reaction of the waste with water was observed, and temperature change was measured with a thermometer while qualitatively observing solubility of the waste sample.
Corrosivity, the pH was determined by visual comparison of pH paper color plates.
And oxidizing, namely putting the sample on a potassium iodide starch test strip, and if KI is oxidized, the generated iodine simple substance shows dark blue when meeting starch, which shows that the oxidizing test result is positive.
Polymerizability, the sample reacts with triethylamine and is judged by temperature change.
Sulfide, under acidic conditions, can generate hydrogen sulfide and turn the lead acetate paper to a silver brown or black color.
Cyanide, contained cyanide is acidified to release hydrogen cyanide gas, so that the cyanide test paper changes color, and judgment is carried out through the color change.
Flammability, heating and burning a waste sample, and judging flammability based on the observed phenomenon.
The invention has the following beneficial effects:
1. the method can analyze 7 indexes of corrosivity, oxidability, polymerizability, water compatibility, cyanide, sulfide and flammability at one time, can basically know the hazard characteristics of the waste, is convenient to set the transportation and storage modes of the waste, and has a guiding function on the subsequent treatment process of the waste;
2. the method needs a small amount of reagents and samples, and does not need a plurality of experimental steps and reagent preparation processes;
3. the method can quickly perform qualitative analysis on the waste, and the pretreatment and test processes are simple;
4. the method has small investment, does not need to use complex and precise large-scale equipment, and is provided with simple glassware and a heating device.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The hazardous waste is usually in the form of liquid, solid, non-liquid or other sample, and the sample is pretreated (except for flammability test) as follows:
for aqueous samples, the analysis was performed "as is".
For samples in solid, non-liquid or other forms, the samples were prepared as follows:
a) add 1mL or 1g of sample to the tube or beaker and remove 10mL of water into the tube or beaker and mix well.
b) The suspension was allowed to settle by standing.
Prepare 3 tubes, take out three uniform samples, and pretreat them as required. First, the various reactions observed were observed to be recorded: smoking, gassing, precipitation, creaminess, etc. If any of the above reactions occur, this indicates that the sample failed the water compatibility test. If no reaction is observed, nor is there a significant temperature change, the waste sample passes the water compatibility test. No reactivity was recorded. The solubility of the waste was recorded as soluble, partially soluble, insoluble.
Dropping one or more drops of the sample solution onto a pH test paper, judging and recording the pH value of the solution, and judging the pH value of the sample.
Simultaneously, a drop of the pretreated sample solution was dropped onto a potassium iodide starch test paper using a clean dropper. Within one minute, the test paper turned blue, indicating a positive result of the oxidation test. Otherwise, it is negative.
2mL of triethylamine was directly added to the tube, mixed well, immediately inserted into a thermometer, and the temperature of the solution at this time was recorded. Observing whether reactions such as temperature rise, air release, polymerization, gel and the like occur. Note that if fine bubbles are observed rising above the liquid level, gas evolution is indicated. If any of the above reactions occurred, the sample failed the polymerizability test and the reason for the failure was recorded. If no reaction occurred, this indicates that the sample's polymerizability test passed.
Another pretreated sample was added slowly to 5mL of hydrochloric acid (1+1) and mixed well. The lead acetate test paper was wetted and attached to the inner wall of the container, taking care not to come into contact with the sample. The lead acetate paper turns silver brown or black to indicate that sulfide exists in the sample, and the test result is recorded as positive. The lead acetate test paper does not change color, and the test result is recorded as negative.
And taking another pretreated sample, acidifying the sample by using a sulfuric acid solution, and slowly mixing to regulate the strong acidity. Placing a piece of cyanide test paper in a test tube opening, enabling the bottom of the test paper to be above the liquid level, and enabling the other part of the test paper to extend out of the test tube opening, and taking care not to immerse the test paper into the solution; the test tube mouth was immediately plugged with a stopper and placed in a water bath at 70 ℃. Checking the cyanide test paper for color change; if the test paper turns blue, indicating that cyanide exists, recording that the cyanide test result is positive.
And (3) performing flammability test, namely directly putting 4ml or 4g of sample into an aluminum weighing boat, igniting a gas torch, and adjusting to a blue flame which is not easy to extinguish, wherein the best state is a sharp blue flame. Note that the flame of the gas torch does not touch the sample. If ignition (flashing or burning) is observed, a conclusion can be drawn that it is flammable. If not, the test is continued. A flame was placed on the sample for at least 15 seconds to ignite the sample. If the sample is ignited, the flammability test result may be judged to be positive. If the sample decomposes, boils (e.g., liquid) or is not ignited by continuous heating with a lamp flame for 15 seconds, a negative flammability test result may be reported.
And (3) judging the hazard characteristics:
a) if the pH value is less than 4 or greater than 10, the pH value is determined to be acidic and corrosive;
b) is determined to be "water compatible" if not reactive with water;
c) if the oxidability test is positive, determining that the product has oxidability;
d) if the test of polymerizability is positive, determining that the polymer is 'polymerizability';
e) if the cyanide and sulfide test is positive, the cyanide and sulfide are determined to be "cyanide" and "sulfide";
f) if the flammability test is positive, then it is determined to be "flammable";
g) whether the waste sample is "dangerous" is finally determined according to the above description of the dangerous characteristics.
Compared with the prior art, the method can analyze 7 indexes of corrosivity, oxidability, polymerizability, water compatibility, cyanide, sulfide and flammability at one time, can basically know the hazard characteristics of the waste, is convenient to set the transportation and storage modes of the waste, and has a guiding function on the subsequent treatment process of the waste; the method needs a small amount of reagents and samples, and does not need a plurality of experimental steps and reagent preparation processes; the method can quickly perform qualitative analysis on the waste, and the pretreatment and test processes are simple; the method has small investment, does not need to use complex and precise large-scale equipment, and is provided with simple glassware and a heating device.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for rapidly detecting hazardous characteristics of hazardous waste is characterized by sequentially comprising the following steps:
s1, mixing a sample with water in a container, and observing whether a reaction occurs or not;
s2, if no reaction exists, recording the solubility as soluble, partially soluble and insoluble according to the solubility;
s3, dripping one or more drops of sample solution onto pH test paper, judging and recording the pH value of the solution, and judging the pH value of the sample;
s4, dripping one or a plurality of drops of sample solution on potassium iodide starch test paper, wherein if the test paper is blue, the oxidation test result is positive, otherwise, the oxidation test result is negative;
s5, adding triethylamine into a part of sample solution, uniformly mixing, immediately inserting a thermometer, recording the temperature of the solution at the moment, and if any one or more of temperature rise, air release, polymerization and gelation occur, judging that the polymerizability is positive, otherwise, judging that the polymerizability is negative;
s6, adding a hydrochloric acid solution into a part of sample solution, fully mixing, wetting lead acetate test paper, enabling the lead acetate test paper to be attached to the inner wall of the container and not to be in contact with the sample solution, if the lead acetate test paper is changed into silver brown or black, judging that the result of sulfide in the sample is positive, otherwise, judging that the result is negative;
s7, adding a sulfuric acid solution into a part of sample solution for acidification, slowly adjusting the mixed solution to be strongly acidic, placing a cyanide test paper on a container opening, enabling the bottom of the test paper to be above the liquid level, enabling the other part of the test paper to extend out of the container opening and not to be in contact with the sample solution, immediately plugging the container opening by using a plug, placing the container opening into a water bath at 70 ℃, if the middle of the test paper turns blue, judging that the result of the cyanide in the sample is positive, otherwise, judging that the result is negative;
s8, putting a sample into an aluminum weighing boat, igniting a gas torch, adjusting to a blue flame which is not easy to extinguish, wherein the flame of the gas torch does not contact the sample, judging that the sample has inflammability if an ignition phenomenon is observed, continuing to test if the sample is not ignited, putting the flame on the sample for at least 15 seconds, judging that the flammability test result is positive if the ignition phenomenon is observed, and judging that the flammability result is negative if the sample is decomposed, boiled or continuously heated by lamp flame for 15 seconds and is not ignited;
s9, result evaluation:
a) if the pH value is less than 4 or greater than 10, the pH value is determined to be acidic and corrosive;
b) is determined to be "water compatible" if not reactive with water;
c) if the oxidability test is positive, determining that the product has oxidability;
d) if the test of polymerizability is positive, determining that the polymer is 'polymerizability';
e) if the cyanide and sulfide test is positive, the cyanide and sulfide are determined to be "cyanide" and "sulfide";
f) if the flammability test is positive, then it is determined to be "flammable";
g) whether the waste sample is "dangerous" is finally determined according to the above description of the dangerous characteristics.
2. The method for rapidly detecting the hazardous property of hazardous waste according to claim 1, wherein the mass-to-volume ratio or the volume ratio of the sample to the water in step S1 is 1: 10.
3. The method for rapidly detecting hazardous characteristics of hazardous waste according to claim 1, wherein said observing whether to react in step S1 is to determine whether smoke, gas release, precipitation, emulsion and obvious temperature change occur, if any one or more of them occur, then it is determined to be reacted, otherwise, it is determined not to be reacted.
4. The method for rapidly detecting hazardous characteristics of hazardous waste according to claim 1, wherein the volume ratio of the triethylamine to the sample solution in step S5 is 1: (0.8-1.5).
5. The method for rapidly detecting hazardous characteristics of hazardous waste according to claim 1, wherein the hydrochloric acid solution is prepared by uniformly mixing concentrated hydrochloric acid and water in a volume ratio of 1:1 in step S6.
6. The method for rapidly detecting hazardous characteristics of hazardous waste according to claim 1, wherein the volume ratio of the hydrochloric acid solution to the sample solution in step S6 is 5: (3-5).
7. The method for rapidly detecting the hazardous property of hazardous waste according to claim 1, wherein the strongly acidic pH value in step S7 is 1-2.
8. The method for rapidly detecting hazardous characteristics of hazardous waste of claim 1, wherein said ignition phenomenon in step S8 comprises flashing or burning.
9. The method for rapidly detecting the hazardous characteristics of hazardous waste according to claim 1, wherein the container is a test tube, a beaker or a flask.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010089949.9A CN111239323A (en) | 2020-02-13 | 2020-02-13 | Rapid detection method for hazardous waste hazard characteristics |
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| CN202010089949.9A CN111239323A (en) | 2020-02-13 | 2020-02-13 | Rapid detection method for hazardous waste hazard characteristics |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121080A (en) * | 1991-06-28 | 1996-04-24 | 埃克森化学专利公司 | Immobilized lewis acid catalysts |
| CN102585709A (en) * | 2007-08-08 | 2012-07-18 | 日立化成工业株式会社 | Adhesive composition, film-like adhesive and connection structure for circuit member |
| CN105606599A (en) * | 2015-09-11 | 2016-05-25 | 山东省食品药品检验研究院 | Rapid detection kit and detection method for cyanide in Chinese liquor |
| CN109991372A (en) * | 2019-03-26 | 2019-07-09 | 陈曦 | Small all-in-one dangerization danger waste classifying calibration method and equipment |
-
2020
- 2020-02-13 CN CN202010089949.9A patent/CN111239323A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121080A (en) * | 1991-06-28 | 1996-04-24 | 埃克森化学专利公司 | Immobilized lewis acid catalysts |
| CN102585709A (en) * | 2007-08-08 | 2012-07-18 | 日立化成工业株式会社 | Adhesive composition, film-like adhesive and connection structure for circuit member |
| CN105606599A (en) * | 2015-09-11 | 2016-05-25 | 山东省食品药品检验研究院 | Rapid detection kit and detection method for cyanide in Chinese liquor |
| CN109991372A (en) * | 2019-03-26 | 2019-07-09 | 陈曦 | Small all-in-one dangerization danger waste classifying calibration method and equipment |
Non-Patent Citations (1)
| Title |
|---|
| 杨菲 等: "危险废物处置企业实验室快速分析能力建设初探", 《探索科学》 * |
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Application publication date: 20200605 |