A method for digesting and detecting geological sample soil

Abstract

The invention belongs to the technical field of geological sample detection, and specifically relates to a digestion and detection method for geological sample soil. The digestion and detection method comprises the following steps: step S1: accurately weighing 0.2500g of sample and placing it in a 50mL beaker, wetting the sample with a small amount of distilled water, and sequentially adding 5.0mL of nitric acid, 2.0mL of phosphoric acid, 5.0mL of hydrofluoric acid and 1.0mL of perchloric acid; step S2: placing the beaker on an electric heating plate, heating the electric heating plate to 120°C, heating the beaker with the sample for 120 minutes, then turning off the electric heating plate and leaving it overnight; step S3: then turning on the electric heating plate, heating and decomposing the sample in the beaker at 180-220°C, and evaporating until white smoke is exhausted, until the sample is completely digested; step S4: turning off the power of the electric heating plate. The present invention adopts a soil digestion and detection method, and uses four-acid open digestion inductively coupled plasma emission spectrometry (ICP-AES) to determine 13 elements such as total sulfur, total phosphorus, and total arsenic in geochemical samples. The 13 elements in the soil can be detected simultaneously, thereby improving the soil detection efficiency and accuracy.

Description

Technical Field

[0001] The invention relates to the technical field of geological sample detection, and in particular to a method for digesting and detecting geological sample soil. Background Art

[0002] Geological samples are various mineral products produced in the earth's crust. They are materials with calibration functions after being tested by authoritative laboratories. The raw material standard samples include: soil, calcium carbonate, cement, coal, coal ash, coke, copper ore, solder, glass, lead, manganese, molybdenum, nickel, multi-element oxides, refractory materials, zircon, silica, slag, slag, steel slag, sludge, tungsten powder, lubricating oil, catalyst, etc. Soil digestion is to release the nutrients, metal ions and other substances you need to measure from these organic-inorganic complexes, so as to accurately measure the substances you need to measure in the soil.

[0003] Existing element detection in geological sample soil generally adopts multi-batch detection, for example, the content of manganese, nitrogen, sulfur, fluorine, sun and other elements is detected in turn, and the content of corresponding elements in the soil is detected in batches in turn. However, this is time-consuming and labor-intensive. Even if some detection methods can detect multiple elements at the same time, the number of detections at one time is limited. At present, there is still a lack of a detection method that can detect more elements in the soil at the same time, so as to improve the detection efficiency and accuracy. Summary of the invention

[0004] The present invention aims to solve one of the technical problems existing in the prior art or related technology.

[0005] To this end, the technical solution adopted in the present invention is:

[0006] A method for digesting and detecting geological sample soil, the method comprising the following steps:

[0007] Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence;

[0008] Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight;

[0009] Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 180-220°C, evaporate until white smoke disappears, and until the sample is completely digested;

[0010] Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 5 h to 8 h, and then measure it on an inductively coupled plasma spectrometer.

[0011] In a preferred example, the present invention can be further configured as follows: in step S2, if the sample is not completely decomposed, nitric acid and hydrofluoric acid can be added before it is completely evaporated until the sample is completely digested.

[0012] In a preferred example, the present invention can be further configured as follows: the setting parameters of the inductively coupled plasma spectrometer are as follows:

[0013] Vertical observation height 15mm

[0014] Transmitting power: 1350w

[0015] Peristaltic pump speed 50r / min

[0016] Carrier gas pressure 0.30MPa

[0017] Shortwave integration time 10s

[0018] Long wave integration time 5s.

[0019] In a preferred example, the present invention can be further configured as follows: the wavelength of the element to be measured of the inductively coupled plasma spectrometer is selected as follows:

[0020] S 182.034nm

[0021] B 208.959nm

[0022] As 189.042nm

[0023] Ca 317.933nm

[0024] Cr 267.716nm

[0025] Cu 327.396nm

[0026] K 766.490nm

[0027] Mg 285.213nm

[0028] Na 589.592nm

[0029] Ni 231.604nm

[0030] Pb 220.353nm

[0031] V 310.230nm

[0032] Zn 213.856nm.

[0033] In a preferred example, the present invention can be further configured as follows: in step S2, the beaker is placed in a ventilated place overnight.

[0034] In a preferred example, the present invention can be further configured as follows: in step S2, the overnight placement time is 8-12 hours.

[0035] In a preferred example, the present invention can be further configured as follows: in step S4, the deionized water is used to rinse the cup wall using a laboratory pressure rinser.

[0036] In a preferred example, the present invention can be further configured as follows: the beaker and the test tube are both made of polytetrafluoroethylene structure.

[0037] The above technical solution of the present invention has the following beneficial technical effects:

[0038] The present invention adopts a soil digestion and detection method, and uses four-acid open digestion inductively coupled plasma emission spectrometry (ICP-AES) to determine 13 elements such as total sulfur, total phosphorus, and total arsenic in geochemical samples. The 13 elements in the soil can be detected simultaneously, thereby improving the soil detection efficiency and accuracy. DETAILED DESCRIPTION

[0039] To make the purpose, technical solution and advantages of the present invention more clear, the present invention is further described in detail below in conjunction with specific implementation methods. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

[0040] It is to be understood that these descriptions are exemplary only and are not intended to limit the scope of the invention.

[0041] The following describes a method for digesting and detecting geological sample soil provided by some embodiments of the present invention.

[0042] Embodiment 1:

[0043] The present invention provides a method for digesting and detecting geological sample soil, the method comprising the following steps:

[0044] Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence;

[0045] Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight;

[0046] Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 180-220°C, evaporate until white smoke disappears, and until the sample is completely digested;

[0047] Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 5 h to 8 h, and then measure it on an inductively coupled plasma spectrometer.

[0048] Specifically, in step S2, if the sample is not completely decomposed, nitric acid and hydrofluoric acid may be added before the sample is completely evaporated until it is completely digested.

[0049] Specifically, the setting parameters of the inductively coupled plasma spectrometer are as follows:

[0050] Vertical observation height 15mm

[0051] Transmitting power: 1350w

[0052] Peristaltic pump speed 50r / min

[0053] Carrier gas pressure 0.30MPa

[0054] Shortwave integration time 10s

[0055] Long wave integration time 5s.

[0056] Specifically, the wavelength of the element to be measured by the inductively coupled plasma spectrometer is selected as follows:

[0057] S 182.034nm

[0058] B 208.959nm

[0059] As 189.042nm

[0060] Ca 317.933nm

[0061] Cr 267.716nm

[0062] Cu 327.396nm

[0063] K 766.490nm

[0064] Mg 285.213nm

[0065] Na 589.592nm

[0066] Ni 231.604nm

[0067] Pb 220.353nm

[0068] V 310.230nm

[0069] Zn 213.856nm.

[0070] Specifically, in step S2, the beaker is placed in a ventilated place overnight.

[0071] Specifically, in step S2, the overnight storage time is 8-12 hours.

[0072] Specifically, in step S4, the deionized water is used to rinse the cup wall using a laboratory pressure rinser, so that less than 25 ml of deionized water can clean the cup wall to prevent element residue.

[0073] Specifically, the beaker and the test tube are both made of polytetrafluoroethylene.

[0074] Specifically, the present application uses four-acid open digestion inductively coupled plasma optical emission spectrometry (ICP-AES) to determine 13 elements such as total sulfur, total phosphorus, and total arsenic in geochemical samples.

[0075] Embodiment 2:

[0076] A method for digesting and detecting geological sample soil, the method comprising the following steps:

[0077] Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence;

[0078] Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight;

[0079] Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 200°C, evaporate until the white smoke disappears, and until the sample is completely digested;

[0080] Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 6 hours, and then measure it on an inductively coupled plasma spectrometer.

[0081] Furthermore, in step S2, if the sample is not completely decomposed, nitric acid and hydrofluoric acid may be added before the sample is completely evaporated to dryness until the sample is completely digested.

[0082] Furthermore, the setting parameters of the inductively coupled plasma spectrometer are as follows:

[0083] Vertical observation height 15mm

[0084] Transmitting power: 1350w

[0085] Peristaltic pump speed 50r / min

[0086] Carrier gas pressure 0.30MPa

[0087] Shortwave integration time 10s

[0088] Long wave integration time 5s.

[0089] Furthermore, the wavelength of the element to be measured by the inductively coupled plasma spectrometer is selected as follows:

[0090] S 182.034nm

[0091] B 208.959nm

[0092] As 189.042nm

[0093] Ca 317.933nm

[0094] Cr 267.716nm

[0095] Cu 327.396nm

[0096] K 766.490nm

[0097] Mg 285.213nm

[0098] Na 589.592nm

[0099] Ni 231.604nm

[0100] Pb 220.353nm

[0101] V 310.230nm

[0102] Zn 213.856nm.

[0103] Furthermore, in step S2, the beaker is placed in a ventilated place overnight.

[0104] Furthermore, in step S2, the overnight storage time is 8-12 hours.

[0105] Furthermore, in step S4, the cup wall is rinsed with deionized water using a laboratory pressure rinser.

[0106] Furthermore, the beaker and the test tube are both made of polytetrafluoroethylene.

[0107] Embodiment three:

[0108] A method for digesting and detecting geological sample soil, the method comprising the following steps:

[0109] Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence;

[0110] Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight;

[0111] Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 210°C, evaporate until the white smoke disappears, and until the sample is completely digested;

[0112] Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 7 hours, and then measure it on an inductively coupled plasma spectrometer.

[0113] Preferably, in step S2, if the sample is not completely decomposed, nitric acid and hydrofluoric acid may be added before the sample is completely evaporated to dryness until the sample is completely digested.

[0114] Preferably, the setting parameters of the inductively coupled plasma spectrometer are as follows:

[0115] Vertical observation height 15mm

[0116] Transmitting power: 1350w

[0117] Peristaltic pump speed 50r / min

[0118] Carrier gas pressure 0.30MPa

[0119] Shortwave integration time 10s

[0120] Long wave integration time 5s.

[0121] Preferably, the wavelength of the element to be measured by the inductively coupled plasma spectrometer is selected as follows:

[0122] S 182.034nm

[0123] B 208.959nm

[0124] As 189.042nm

[0125] Ca 317.933nm

[0126] Cr 267.716nm

[0127] Cu 327.396nm

[0128] K 766.490nm

[0129] Mg 285.213nm

[0130] Na 589.592nm

[0131] Ni 231.604nm

[0132] Pb 220.353nm

[0133] V 310.230nm

[0134] Zn 213.856nm.

[0135] Preferably, in step S2, the beaker is placed in a ventilated place overnight.

[0136] Preferably, in step S2, the overnight storage time is 8-12 hours.

[0137] Preferably, in step S4, the cup wall is rinsed with deionized water using a laboratory pressurized rinser.

[0138] Preferably, the beaker and the test tube are both made of polytetrafluoroethylene.

[0139] Embodiment 4:

[0140] The present invention provides a method for digesting and detecting geological sample soil, the method comprising the following steps:

[0141] Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence;

[0142] Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight;

[0143] Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 180°C, evaporate until white smoke disappears, and until the sample is completely digested;

[0144] Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 5 hours, and then measure it on an inductively coupled plasma spectrometer.

[0145] It should be noted that in step S2, if the sample is not completely decomposed, nitric acid and hydrofluoric acid can be added before it is completely evaporated to dryness until the sample is completely digested.

[0146] It should be noted that the setting parameters of the inductively coupled plasma spectrometer are as follows:

[0147] Vertical observation height 15mm

[0148] Transmitting power: 1350w

[0149] Peristaltic pump speed 50r / min

[0150] Carrier gas pressure 0.30MPa

[0151] Shortwave integration time 10s

[0152] Long wave integration time 5s.

[0153] It should be noted that the wavelength of the element to be measured by the inductively coupled plasma spectrometer is selected as follows:

[0154] S 182.034nm

[0155] B 208.959nm

[0156] As 189.042nm

[0157] Ca 317.933nm

[0158] Cr 267.716nm

[0159] Cu 327.396nm

[0160] K 766.490nm

[0161] Mg 285.213nm

[0162] Na 589.592nm

[0163] Ni 231.604nm

[0164] Pb 220.353nm

[0165] V 310.230nm

[0166] Zn 213.856nm.

[0167] It should be noted that in step S2, the beaker is placed in a ventilated place overnight.

[0168] It should be noted that, in step S2, the overnight storage time is 8-12 hours.

[0169] It should be noted that in step S4, the cup wall is rinsed with deionized water using a laboratory pressure rinser.

[0170] It should be noted that the beaker and the test tube are both made of polytetrafluoroethylene.

[0171] It should be noted that the present application uses four-acid open digestion inductively coupled plasma optical emission spectrometry (ICP-AES) to determine 13 elements such as total sulfur, total phosphorus, and total arsenic in geochemical samples.

[0172] The working principle and use process of the present invention are as follows: firstly, 0.2500 g of a sample is accurately weighed and placed in a 50 mL polytetrafluoroethylene beaker, a small amount of distilled water is used to wet the sample, 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1 mL of perchloric acid are added in sequence, the temperature of an electric heating plate is heated to 120° C., the beaker containing the sample is heated for 120 minutes, the electric heating plate is turned off, and the sample is placed in a fume hood overnight; then the electric heating plate is turned on, the sample is heated and decomposed at 180-220° C., and the sample is evaporated to dryness until white smoke is completely emitted. If the sample is not completely decomposed, add nitric acid and hydrofluoric acid before it is completely evaporated until the sample is completely digested; turn off the power of the hot plate, then add 8.0mL of aqua regia, and continue heating on the hot plate using the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25mL polytetrafluoroethylene color tube, make up to 25mL with deionized water, let it stand for 5h∽8h, and then measure on an inductively coupled plasma spectrometer.

[0173] In the description of this specification, the description of the terms "one embodiment", "some embodiments", "specific embodiments", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0174] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A method for digesting and detecting geological sample soil, characterized in that: The digestion and detection method comprises the following steps: Step S1: Accurately weigh 0.2500 g of sample and place it in a 50 mL beaker, wet the sample with a small amount of distilled water, and add 5.0 mL of nitric acid, 2.0 mL of phosphoric acid, 5.0 mL of hydrofluoric acid and 1.0 mL of perchloric acid in sequence; Step S2: placing the beaker on a hot plate, heating the hot plate to 120° C., heating the beaker containing the sample for 120 minutes, then turning off the hot plate and leaving it overnight; Step S3: Then turn on the electric heating plate, heat and decompose the sample in the beaker at 180-220° C., evaporate until white smoke disappears, and until the sample is completely digested. If the sample is not completely decomposed, add nitric acid and hydrofluoric acid before it is completely evaporated until the sample is completely digested; Step S4: Turn off the power of the hot plate, then add 8.0 mL of aqua regia, continue to heat on the hot plate with the residual heat until the salts are completely dissolved and the solution is clear, rinse the cup wall with deionized water, transfer the solution to a 25 mL test tube, add deionized water to make the volume 25 mL, let it stand for 5 h to 8 h, and then measure it on an inductively coupled plasma spectrometer; The setting parameters of the inductively coupled plasma spectrometer are as follows: Vertical observation height 15mm Transmitting power: 1350w Peristaltic pump speed 50r / min Carrier gas pressure 0.30MPa Shortwave integration time 10s Long wave integration time 5s; The wavelength of the element to be measured by the inductively coupled plasma spectrometer is selected as follows: S182.034nm B 208.959nm As 189.042nm Ca 317.933nm Cr 267.716nm Cu 327.396nm K 766.490nm Mg 285.213nm Na 589.592nm Ni 231.604nm Pb 220.353nm V 310.230nm Zn 213.856nm.

2. The method for digesting and detecting geological sample soil according to claim 1, characterized in that: In step S2, the beaker is placed in a ventilated place overnight.

3. The method for digesting and detecting geological sample soil according to claim 1, characterized in that: In step S2, the overnight storage time is 8-12 hours.

4. The method for digesting and detecting geological sample soil according to claim 1, characterized in that: In step S4, the cup wall is rinsed with deionized water using a laboratory pressure rinser.

5. The method for digesting and detecting geological sample soil according to claim 1, characterized in that: The beaker and the test tube are both made of polytetrafluoroethylene.