CN110455700B - Small-diameter thin-walled tube hydrogen induced cracking test method and evaluation method - Google Patents
Small-diameter thin-walled tube hydrogen induced cracking test method and evaluation method Download PDFInfo
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Abstract
A small-diameter thin-walled tube hydrogen induced cracking test method and an evaluation method thereof are disclosed, wherein the test method comprises the following steps: s1, cutting the small-diameter thin wall into a plurality of annular pipe sections along the length direction to be used as original sample pipes; s2, measuring the geometric dimension of each sample original tube before testing, and carrying out degreasing treatment; s3, placing the original sample tube into a sample container, and fixing the original sample tube; s4, carrying out test treatment on the sample in a test container, and recording the surface condition of the sample original tube after the test treatment; s5, obtaining a metallographic surface; s6, marking each crack and calculating the crack rate. The invention solves the problems that the sample is difficult to manufacture and the metallographic examination surface is difficult to prepare; defining a hydrogen induced cracking crack identification method and a crack size measurement method of a small-diameter thin-wall steel pipe; and (3) carrying out tests and crack statistics on the steel pipes which are not in the standard application range by referring to the test method of the invention, so that the steel pipes are applicable to the existing standard evaluation system.
Description
Technical Field
The invention relates to the field of material detection, in particular to a small-diameter thin-wall tube hydrogen induced cracking test method and an evaluation method.
Background
Along with the rapid development of national economy, the demand of energy is more and more large, the national requirements on environmental protection are higher and more, the energy structure is gradually changed, the consumption of petroleum and natural gas is increased year by year, and the trend of replacing coal to become main energy is high. The usage amount of the pipeline steel as a main transportation carrier of petroleum and natural gas resources is increased year by year, but with the development of oil and gas fields and the continuous increase of the processing amount of imported high-sulfur crude oil, the corrosion damage of a hydrogen sulfide medium has penetrated into the drilling, transportation and processing industries of petroleum and natural gas. More and more pipelines are subject to corrosion cracking in a wet hydrogen sulfide environment. The hydrogen induced Cracking is the most common one of the Corrosion Cracking, relevant detection standards are established for the hydrogen induced Cracking in various countries, and the most widely applied hydrogen induced Cracking inspection standards in China at present mainly comprise GB/T8650-2015 evaluation method for hydrogen induced Cracking Resistance of pipeline steel and pressure vessel steel and NACE TM0284-2016Laboratory Testing of Metals for Resistance to Stress crack Cracking and Stress crack Cracking H2S Environments, the application range of the S Environments to small-diameter pipes is resistance welding and seamless steel pipes with the nominal diameter of DN 50-150 mm and the wall thickness of less than or equal to 6mm, and the current standard of the steel pipes with the diameter of less than 50mm does not specify how to carry out a hydrogen induced cracking test. The heat exchange tube is used as a main component in a heat exchanger, a small-diameter thin-wall steel tube is generally used, the pipeline steel is just not in the application range of the hydrogen induced cracking test standard, and the related technical documents generally require the hydrogen induced cracking of the steel tube with reference to GB/T8650 or NACE TM0284And (4) performing a cracking test. The existing technical scheme can not truly reflect the corrosion condition of a hydrogen induced cracking sample, and the test result is smaller than the actual result, so that the potential safety hazard occurs in the safe long-period operation of petrochemical equipment.
The identification of the cracks and the geometric sizes of the cracks have obvious influence on the hydrogen induced cracking test results of the small-diameter thin-wall steel pipe. The existing hydrogen induced cracking test standard stipulates that 'cracks within 1mm of the upper surface and the lower surface of a test sample are not counted as hydrogen induced cracking cracks', the evaluation of the hydrogen induced cracking test result of the thin-wall steel pipe is obviously influenced, the wall thickness of the thin-wall steel pipe test sample is originally thin, the removal of the cracks within 1mm of the inner wall and the outer wall is not counted as the hydrogen induced cracking cracks, and the use risk of the thin-wall steel pipe can be greatly enlarged. For example, for a heat exchange tube sample with the wall thickness of 2.5mm, oxide skins on the inner wall and the outer wall are removed, the actually measured wall thickness of the sample is close to 2mm, cracks within 1mm of the inner wall and the outer wall do not participate in the calculation of the crack rate after the test, so that the hydrogen induced cracking performance test is basically not needed for the steel tube with the wall thickness of less than or equal to 2.5mm, and even if cracks exist, the cracks are probably not recognized as hydrogen induced cracking cracks under the existing regulation, which is a great hidden danger under the safe long-period operation burying of equipment. The hydrogen induced cracking of the small-diameter thin-wall steel pipe is subject to the self regulation, and the formation mechanism of the hydrogen bubbling on the surface of the sample and the hydrogen induced cracking inside the sample is consistent, so that the cracks formed by the hydrogen bubbling on the surface of the sample are also the hydrogen induced cracking cracks.
Hydrogen-induced cracking cracks in steel pipes are somewhat different from hydrogen-induced cracking cracks in steel plates, which may appear irregular. Irregular cracks are closely related to the placing positions of samples in the aspect of geometric dimension measurement, the geometric dimension difference of the cracks is obvious when the same crack is observed at different viewing angles, the thin-wall pipe fitting is very sensitive to the crack thickness rate, the definition of the length and the thickness of the crack can influence the judgment of a final result, and no unified regulation is provided for reference execution aiming at the definition of the length and the thickness of the hydrogen induced crack of the small-diameter thin-wall pipe.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a small-diameter thin-wall tube hydrogen induced cracking test method and an evaluation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
s1, removing an oxide layer or a rust layer from the small-diameter thin-walled tube through outer wall and inner wall treatment, ensuring the set wall thickness and surface roughness of the small-diameter thin-walled tube, and then cutting the small-diameter thin-walled tube into a plurality of annular tube sections with unit length along the length direction or cutting the annular tube sections axially to obtain arc sections serving as original sample tubes;
s2, measuring the geometric dimension of each sample original tube before testing, and carrying out degreasing treatment;
s3, placing the original sample tubes into a test container, wherein the mutual interval between the original sample tubes is not less than a set distance, and fixing the original sample tubes;
s4, performing a hydrogen induced cracking corrosion test on the sample in a test container, taking out the sample original tube after the test is finished, cleaning and drying the sample original tube, photographing, and recording the surface condition of the sample original tube after corrosion;
s5, obtaining a metallographic surface, and when the original sample pipe is a base material or a straight welding line, equally dividing the original sample pipe into multiple parts in the length direction, wherein the equally divided surfaces are used as metallographic examination surfaces; when the original sample pipe is an annular welding seam sample, performing N equal division on the annular welding seam sample in the length direction to form N welding seam sample subsections; the upper surfaces of the two end surfaces of each welding seam sample subsection after horizontal cutting are used as metallographic examination surfaces, and the distance from each metallographic examination surface to the upper surface of the corresponding welding seam sample subsection is different;
and S6, marking each crack on the metallographic examination surface.
The method for evaluating the data acquired after the small-diameter thin-walled tube hydrogen induced cracking test method comprises the following steps of:
s7, setting the direction parallel to the neutral layer (102) of the original sample tube as the length direction of the crack (104), setting the direction perpendicular to the neutral layer (102) of the original sample tube as the thickness direction of the crack (104), aligning a microscope to the position of the crack (104), converting the scanning field of view of the original base material or the straight welding seam sample by rotating the original sample tube to obtain the corresponding size of each crack (104), and uniformly calculating the circumferences of arcs where different cracks (104) are located by taking the circumference of the neutral layer (102) as a calculation basis;
s8, calculating the single check surface crack rate, wherein the calculation formula is as follows:
wherein a represents the length of the crack (104), b represents the thickness of the crack (104), the perimeter of the neutral layer (102) of the sample original pipe is represented for the base material or the straight welding line L, and T represents the wall thickness of the sample original pipe; for the girth weld sample, L represents the length of the sample original pipe inspection surface 212, and T represents the width of the sample inspection surface 212 overlapping with one side wall of the steel pipe.
The invention has the advantages that:
(1) the invention carries out the hydrogen induced cracking test in a mode of splitting the whole annular pipe or the arc section obtained by diameter, and solves the problems that the sample is difficult to manufacture and the metallographic examination surface is difficult to obtain compared with the boat-shaped sample in GB/T8650-2015 standard which needs to be set in width.
(2) The invention establishes a new rule aiming at the identification of the hydrogen-induced cracking crack of the small-diameter thin-wall steel pipe, and the formation mechanism of the hydrogen blister on the surface of the sample and the hydrogen-induced cracking crack in the sample is consistent.
(3) The invention provides a method for defining the crack length and the crack thickness according to the steps S7 and S8. The method eliminates the change of the geometric dimension of the crack caused by the visual angle conversion, in the actual operation process, the microscope objective can be aligned to the position of the crack, the scanning field of view is converted by rotating the base material or the straight welding seam sample instead of translating the sample, the obtained crack length and the crack thickness are very easy to determine, and the influence of radian is not considered in the measurement of the crack dimension in the field of view amplified by 100 times. Because the steel pipe is a thin-wall steel pipe, the circumferential arc lengths of different cracks are not equal and are not considered, and the circumference of a neutral layer is uniformly measured.
(4) Although the inspection range is enlarged, the possibility of finding cracks is improved, and the inspection result is more practical, thereby providing basic guarantee for the safe long-period operation of petrochemical equipment.
(5) The method defines the crack length and the crack thickness and defines the hydrogen induced cracking cracks of the small-diameter thin-wall steel pipe, enlarges the inspection range and has more comprehensive inspection.
Drawings
FIG. 1 is a schematic view showing the position of a metallographic examination surface when a sample parent tube is a base material.
FIG. 2 is a schematic diagram of the position of a metallographic examination surface when the sample original tube is a weld sample.
Fig. 3 is a schematic view of crack geometry definition.
The notations in the figures have the following meanings:
11-parent Material 12/212-metallographic examination surface
21-weld specimen 211-weld 213-specimen section
101-outer wall 102-neutral layer 103-inner wall 104-crack
Detailed Description
Example 1
The small-diameter thin-walled tube hydrogen induced cracking test method comprises the following steps:
s1, removing an oxide layer or a corrosion layer from the small-diameter thin-walled tube through treatment of the outer wall 101 and the inner wall 103, ensuring the set wall thickness of the small-diameter thin-walled tube, and then cutting the small-diameter thin-walled tube into 3 annular tube sections with the unit length of 100 +/-1 mm along the length direction to serve as original sample tubes; the 3 samples were labeled 10(HSC) -HIC-11, 10(HSC) -HIC-12, 10(HSC) -HIC-13, respectively.
In the scheme, the small-diameter thin-wall pipe is a 10(HSC) steel pipe resistant to hydrogen sulfide corrosion. The specification is phi 25 x 2.5 mm. After finish turning of the inner wall 103 and the outer wall 101, a pipe section with the length of 100 +/-1 mm is cut, and the length direction of the pipe section is along the rolling direction of the steel pipe. And grinding the surface of the sample in one direction by using 320# sandpaper to form a sample original tube. The outer wall 101 is finished by a lathe and then ground with sandpaper, and the inner wall 103 is processed by boring, grinding, blasting, or the like. After treatment, the thickness of the original sample tube is at least 80% of the thickness of the small-diameter thin-wall tube.
S2, measuring the geometric dimension of each sample original tube before the experiment, and carrying out degreasing treatment; the degreasing is performed by placing the sample raw tube into an ultrasonic cleaning machine for ultrasonic cleaning, wherein a degreasing agent is arranged in the ultrasonic cleaning machine, and in the embodiment, the degreasing agent comprises acetone and absolute ethyl alcohol.
S3, placing the original sample tubes into the sample container, wherein the mutual interval between the original sample tubes is not less than the set distance, the set distance is not less than 6mm, fixing the original sample tubes, and ensuring sufficient convection of the test solution.
S4, carrying out test treatment on the sample in the test container, taking out the sample original tube, cleaning, drying, photographing, and recording the surface condition of the sample original tube after test treatment;
the test treatment of the sample is carried out according to the specification of NACE TM0284, and comprises the following specific steps:
s41, sealing the container, injecting high-purity nitrogen into the container, wherein the flow rate of the high-purity nitrogen is at least 100mL/min per liter of volume, the time is at least 1h, and the volume of the sample container is controlled within 10L as much as possible;
s42, preparing a solution required by the test, wherein the solution adopts a solution A (namely 5% NaCl + 0.5% CH) specified by a standard3COOH), recording the initial pH of the solution, wherein the initial pH is 2.7 +/-0.1, placing the solution in a sealed solution preparation container, introducing high-purity nitrogen into the solution preparation container to remove oxygen for at least 1h, and the flow rate is at least 100mL/min per liter of solution;
s43, introducing the test solution for removing the peroxide in the liquid preparation container into the sample container, wherein the amount of the test solution is equal to that of the sample containerThe ratio of the surface area of the sample is not less than 3mL/cm2After the introduction, the sample container is continuously deoxidized for 1h, and the flow rate is at least 100mL/min per liter of solution;
s44, closing the high-purity nitrogen valve; opening a hydrogen sulfide valve, introducing hydrogen sulfide gas into the sample container and the liquid preparation container at a flow rate of not less than 200mL/min per liter of solution for at least 1h, measuring the hydrogen sulfide content of the solution in the sample container by an iodometry method, wherein the measurement result shows that the concentration of the hydrogen sulfide in the solution is 2657ppm, measuring the pH value of the solution, wherein the result shows 3.1, regulating the flow rate of the hydrogen sulfide to a plurality of bubbles per minute, keeping the hydrogen sulfide gas at a micro-positive pressure for 96h, and measuring the pH value of the solution in the sample container to be 3.8 until the test is finished.
S5, obtaining a metallographic surface, and when the original sample pipe is a base material 11 or a straight welding line, performing quartering on the original sample pipe in the length direction, and taking an equally divided surface as a metallographic examination surface 12; in fig. 1, the specimen is divided into 4 parts, i.e., 3 divided surfaces in the middle can be seen as metallographic surfaces 12 in fig. 1. In summary, the sample raw pipe includes 9 metallographic surfaces 12 regardless of whether it is the base material sample 11 or the straight weld sample. The numbers are 111, 112, 113, 121, 122, 123, 131, 132 and 133 respectively.
S6, 18 cracks 104 were observed in total, including the cracks 104 formed by surface bulging after the sample pipe test treatment, recorded on the metallographic examination surface 12.
The method for evaluating the data acquired after the small-diameter thin-walled tube hydrogen induced cracking test method comprises the following steps:
s7, setting the direction parallel to the neutral layer 102 of the original sample tube as the length direction of the crack 104, setting the direction perpendicular to the neutral layer 102 of the original sample tube as the thickness direction of the crack 104, aligning a microscope at the position of the crack 104, converting the scanning field by rotating the original sample tube, measuring different cracks 104 uniformly by the circumference of the neutral layer 102, and obtaining the corresponding size of each crack 104;
s8, calculating the rate of the single check surface crack 104, wherein the formula is as follows:
wherein a represents the length of the crack 104, b represents the thickness of the crack 104, L represents the perimeter of the neutral layer 102 of the original sample tube, and T represents the thickness of the original sample tube wall; in fig. 3, 2 cracks 104 are taken as an example, and the length is a1 and a2, respectively, and the width is b1 and b2, respectively.
The length and width of each crack 104 was measured and recorded separately in step S6 as shown in table 1, these cracks 104 being completely within 1mm of the inner and outer walls 103, 101 of the test specimen.
TABLE 1
Referring to the requirement of GB/T8650-2015 standard, for a small-diameter thin-wall seamless steel pipe, the thickness of a sample is at least 80% of the pipe wall thickness, and in combination with the requirement on cracks 104 during sample evaluation, the cracks 104 within 1mm of the inner wall 103 and the outer wall 101 cannot be counted as the cracks 104 in the sample, statistics is not performed in the statistical process of the cracks 104, and the evaluation result is shown in Table 2.
TABLE 2
The results of the evaluation of hydrogen induced cracking 104 according to the method defined in the present invention are shown in Table 3:
TABLE 3
From the comparison, the invention expands the inspection range, improves the probability of finding the crack 104, has more comprehensive inspection and is beneficial to the safe and long-term operation of petrochemical equipment in a wet hydrogen sulfide environment.
Example 2
The difference from example 1 is that the sample in this example is a girth weld sample 21. When a metallographic examination surface is obtained, as shown in fig. 2, trisecting the ring weld specimen 21 in the length direction to form three weld specimen subsections, wherein the trisecting surface is a specimen section 213; and (3) taking the upper surface of each weld sample subsection parallel to the axially cut upper surface as a metallographic examination surface 212, namely obtaining 3 metallographic examination surfaces 212. The distances from each metallographic examination surface 212 to the upper surface of the corresponding weld specimen subsection are different, and in the embodiment, the distances from the metallographic examination surface 212 to the upper surface of the corresponding weld specimen subsection are respectively D/4, D/2 and 3D/4. The three samples obtained 9 test surfaces, which are respectively designated as 111, 112, 113, 121, 122, 123, 131, 132 and 133. The weld 211 in the middle of the weld specimen is the joint of the two base materials 11.
All cracks 104 recorded on the metallographic examination surface 212 included cracks 104 formed by surface bulging after the sample tube test treatment.
Calculating the single check surface crack 104 rate, wherein the calculation formula for the girth weld sample is as follows:
wherein a represents the length of the crack (104), b represents the thickness of the crack (104), L represents the length of the original sample pipe inspection surface 212, and T represents the width of the sample inspection surface 212 overlapped with one side wall of the steel pipe;
the invention is not to be considered as limited to the specific embodiments shown and described, but is to be understood to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The method for evaluating the hydrogen induced cracking of the small-diameter thin-walled tube is characterized by comprising the following steps of:
s1, removing an oxidation layer or a corrosion layer from the small-diameter thin-walled tube through treatment of an outer wall (101) and an inner wall (103), ensuring the set wall thickness and surface roughness of the small-diameter thin-walled tube, and then cutting the small-diameter thin-walled tube into a plurality of annular tube sections with unit length along the length direction or cutting the annular tube sections along the axial direction to obtain arc sections serving as original sample tubes;
s2, measuring the geometric dimension of each sample original tube before testing, and carrying out degreasing treatment;
s3, placing the original sample tubes into a test container, wherein the mutual interval between the original sample tubes is not less than a set distance, and fixing the original sample tubes;
s4, performing a hydrogen induced cracking corrosion test on the sample in a test container, taking out the sample original tube after the test is finished, cleaning and drying the sample original tube, photographing, and recording the surface condition of the sample original tube after corrosion;
s5, obtaining a metallographic surface, and when the original sample pipe is a base material (11) or a straight welding line, equally dividing the original sample pipe into multiple parts in the length direction, wherein the equally divided surfaces are used as metallographic examination surfaces; when the original sample pipe is a circular weld sample (21), performing N equal division on the circular weld sample (21) in the length direction to form N sub-sections of the weld sample (21); the upper surfaces of the two end surfaces of each sub-section of the welding seam sample (21) after horizontal cutting are used as metallographic examination surfaces, and the distances from each metallographic examination surface to the upper surface of the corresponding sub-section of the welding seam sample (21) are different;
s6, marking each crack (104) on the metallographic examination surface;
s7, setting the direction parallel to the neutral layer (102) of the original sample tube as the length direction of the crack (104), setting the direction perpendicular to the neutral layer (102) of the original sample tube as the thickness direction of the crack (104), aligning a microscope to the position of the crack (104), converting the scanning field of view of the original base material or the straight weld sample by rotating the original sample tube to obtain the corresponding size of each crack (104), and uniformly setting the circumferences of arcs where different cracks (104) are located and taking the circumference of the neutral layer (102) of the original sample tube as the calculation basis;
s8, calculating the single check surface crack rate, wherein the calculation formula is as follows:
crack length ratio
Crack thickness ratio
Susceptibility to cracking
Wherein a represents the length of the crack (104), b represents the thickness of the crack (104), L represents the perimeter of the neutral layer (102) of the original sample pipe, and T represents the thickness of the original sample pipe for the base material or the straight welding seam; for the girth weld sample, L represents the length of the original sample pipe inspection surface (212), and T represents the width of the original sample pipe inspection surface (212) overlapping with one side wall of the steel pipe.
2. The method for evaluating the hydrogen induced cracking of the small-diameter thin-walled tube according to claim 1, wherein in step S1, the outer wall (101) is processed by a lathe finish turning and then by sanding or sand blasting, and the inner wall (103) is processed by boring, grinding and sand blasting.
3. The method for evaluating the hydrogen induced cracking of the small-diameter thin-walled tube according to claim 2, wherein the thickness of the original sample tube is at least 80% of the thickness of the small-diameter thin-walled tube, and the inner and outer walls are removed by at most 1mm, so as to ensure that the oxide layer or the rust layer is removed cleanly.
4. The method for evaluating hydrogen induced cracking of a small diameter thin walled tube according to claim 1, wherein the steps of the test treatment in step S4 are as follows:
s41, sealing the container, and injecting high-purity nitrogen into the container;
s42, preparing a solution required by the test, recording the initial pH value of the solution, then placing the solution in a sealed solution preparation container, and introducing high-purity nitrogen into the solution preparation container to remove oxygen;
s43, introducing the test solution for removing the peroxide in the liquid preparation container into the sample container, leading the ratio of the amount of the test solution to the surface area of the sample to a set range, and continuously removing the oxygen from the sample container after introduction;
and S44, introducing hydrogen sulfide gas into the sample container, measuring the content of hydrogen sulfide in the solution in the sample container by an iodometry method, recording the pH value of the solution when the hydrogen sulfide is saturated, then regulating the flow of the hydrogen sulfide to be small, keeping the hydrogen sulfide gas at micro-positive pressure, continuing until the test is finished, and recording the pH value of the solution in the sample container when the test is finished.
5. The method for evaluating the hydrogen induced cracking of a small-diameter thin-walled tube according to claim 1, wherein in step S5, when the original tube is a circular weld specimen (21), the distances from the metallographic examination surface to the upper surface of the sub-section of the corresponding weld specimen (21) are M × D/(N +1), wherein M is 1,2,3 … … N, and D is the outer diameter of the sub-section of the weld specimen (21).
6. The method for evaluating the hydrogen induced cracking of a small diameter thin walled tube according to claim 1, wherein the cracks (104) on the metallographic examination surface recorded in step S6 include cracks (104) formed by surface bulging after the sample raw tube test treatment.
7. The method for evaluating the hydrogen induced cracking of a small diameter thin walled tube according to claim 1, wherein the number of the sample raw tubes in each set of tests is 3.
8. The method for evaluating the hydrogen induced cracking of the small-diameter thin-walled tube according to claim 5, wherein the number of the metallographic examination surface of each raw tube is 3.
9. The method for evaluating the hydrogen induced cracking of the small-diameter thin-walled tube according to claim 1, wherein the degreasing in the step S2 is performed by placing the sample raw tube into an ultrasonic cleaning machine, and a degreasing agent is arranged in the ultrasonic cleaning machine.
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