CN111020409B - High-strength microalloyed steel, underwater oil and gas pipeline quick connector and manufacturing method - Google Patents

High-strength microalloyed steel, underwater oil and gas pipeline quick connector and manufacturing method Download PDF

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CN111020409B
CN111020409B CN201911405584.XA CN201911405584A CN111020409B CN 111020409 B CN111020409 B CN 111020409B CN 201911405584 A CN201911405584 A CN 201911405584A CN 111020409 B CN111020409 B CN 111020409B
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CN111020409A (en
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周勇
葛辉
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Suzhou Regham Hengrui Energy Equipment Engineering Co ltd
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Suzhou Lygm Subsea Oil Equipment Tech Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C21D1/28—Normalising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B17/00—Drilling rods or pipes; Flexible drill strings; Kellies; Drill collars; Sucker rods; Cables; Casings; Tubings
    • E21B17/02—Couplings; joints
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L37/00—Couplings of the quick-acting type

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Abstract

The invention discloses a high-strength microalloyed steel, a quick connector of an underwater oil-gas pipeline and a manufacturing method, wherein the manufacturing heating temperature is less than or equal to 1180 ℃, and the heat preservation time is 0.5-1.5 hours/inch; the heating temperature is less than or equal to 1180 ℃; repeatedly upsetting and drawing the steel ingot transversely and longitudinally for three times by adopting a hydraulic machine WHF forging method and a forging hammer FM forging method, wherein the single forging ratio is more than 2, and the temperature in the whole forging process is controlled at 900-1180 ℃; and (3) carrying out heat treatment, namely normalizing at 960 ℃, quenching at 920 ℃, tempering at 610 ℃, and keeping the temperature for 1.0 hour/inch. The forging piece of the rapid connector with the extra-large wall thickness, which is optimally manufactured through the component design, forging and heat treatment processes, has very excellent weldability and low-temperature performance, and solves the problems of complex design structure, complex process, difficult construction, high operation and maintenance cost and the like of deep sea oil and gas production equipment and conveying pipelines caused by the rapid connector produced by the existing material.

Description

High-strength microalloyed steel, underwater oil and gas pipeline quick connector and manufacturing method
Technical Field
The invention belongs to the technical field of ocean oil and gas production equipment, and particularly relates to a high-strength microalloyed steel, an underwater oil and gas pipeline quick connector and a manufacturing method thereof.
Background
A quick connector for ultra-deep sea oil and gas production equipment with an operating water depth of more than 1500 meters and a conveying pipeline belongs to a main body core component. In the prior art, the forging material of the quick connector generally adopts American standard ASTM A182F 22 grade material or common F65 grade material with small wall thickness. The disadvantages are that the weldability of the ASTM A182F 22 grade material is poor, and post-welding heat treatment is required after welding, which causes great difficulty to site construction and greatly increases the cost; the standard F65 microalloyed steel belongs to low-carbon steel and is microalloyed, and the hardenability is poor, namely the microalloyed steel is generally adopted in pipelines in large quantity. The forging piece wall thickness is less than 100mm when the forging piece is applied to pipelines in the field of oil and gas pipelines (oil and gas pipelines for short). When the wall thickness of the forging exceeds 100mm, the weldability limit (carbon equivalent requirement and welding crack sensitivity coefficient) of the forging needs to be comprehensively considered, the strength and the toughness of the forging exceed the material performance limit, instability is generated, the strength and the low-temperature toughness cannot be matched, and the control is extremely difficult. With the use of ordinary F65 grade material, the yield strength at the center of the forging is less than 450MPa with guaranteed impact performance, the same result is also present in some well known deep sea forging manufacturer in italy and no solution has been obtained. After the process is adjusted to ensure that the yield strength of the central position of the forging reaches the requirement of 450MPa, the single lowest Charpy impact test result at the low temperature of-29 ℃ and-46 ℃ has the phenomenon that the requirement is not met, and the deviation of three impact values of the same group is extremely large and has a difference of more than 10 times. The forging made of the ordinary F65-grade material with the small wall thickness causes the complex structure of the whole equipment, the safety coefficient is reduced, the installation and the maintenance are inconvenient, and the later maintenance cost is huge. The forging needs to consider standardization and modularization of product structure design, and the design and selection of material dimension of the forging have to face the challenges of large wall thickness and supercritical state.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a high-strength microalloyed steel, an underwater oil and gas pipeline quick connector and a manufacturing method thereof, wherein a super-large wall thickness (the wall thickness is more than 200mm) quick connector forged piece manufactured through component design, forging and heat treatment process optimization has excellent weldability and low temperature performance, and the problems of complex design structure, complex working procedures, difficult construction, high operation and maintenance cost and the like of deep sea oil and gas production equipment and a conveying pipeline caused by the conventional quick connector produced by materials are solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-strength microalloyed steel is characterized by comprising the following components in parts by weight: c: 0.00-0.12%, Si: 0.20-0.45%, Mn: 1.10-1.40%, P: 0.000-0.015%, S: 0.000 to 0.010 percent, Cr: 0.10-0.50%, Ni: 0.50-0.99%, Mo: 0.15-0.50%, Cu: 0.000 to 0.30%, Ti: 0.000 to 0.025%, Bi: 0.000 to 0.010%, Nb: 0.000 to 0.020%, Al: 0.020 to 0.055%, Sn: 0.000-0.015%, V: 0.000-0.060%, B: 0.0000-0.0005%, Pb: 0.000 to 0.010%, As: 0.000 to 0.020%, Sb: 0.000 to 0.020%, Ca: 0.000 to 0.005 percent, the balance of Fe, and the carbon equivalent Ce is less than 0.43.
In a specific embodiment of the present invention, the high strength microalloyed steel has a weight composition comprising: c: 0.08-0.10%, Si: 0.20-0.40%, Mn: 1.15-1.30%, P: 0.005-0.015%, S: 0.001-0.006%, Cr: 0.10-0.30%, Ni: 0.60-0.90%, Mo: 0.20-0.30%, Cu: 0.060 to 0.20%, Ti: 0.000 to 0.009%, Bi: 0.000 to 0.0017%, Nb: 0.000 to 0.005%, Al: 0.020 to 0.040%, Sn: 0.001-0.010%, V: 0.000 to 0.040%, B: 0.0001-0.0004%, Pb: 0.000 to 0.0015%, As: 0.001 to 0.005%, Sb: 0.000 to 0.003%, Ca: 0.000 to 0.001 percent, the balance of Fe, and the carbon equivalent Ce is less than 0.43.
The invention also aims to provide the quick connector for the underwater oil-gas pipeline, which is characterized in that the quick connector for the underwater oil-gas pipeline is prepared by taking the high-strength microalloyed steel as a raw material; the quick connector forging is used for ultra-deep sea oil and gas production equipment with the operating water depth of more than 1500 meters and a conveying pipeline.
The invention also aims to provide a manufacturing method of the quick connector of the underwater oil-gas pipeline, which is characterized by comprising the following process steps:
A) the steel ingot comprises the following components in parts by weight: c: 0.00-0.12%, Si: 0.20-0.45%, Mn: 1.10-1.40%, P: 0.000-0.015%, S: 0.000 to 0.010 percent, Cr: 0.10-0.50%, Ni: 0.50-0.99%, Mo: 0.15-0.50%, Cu: 0.000 to 0.30%, Ti: 0.000 to 0.025%, Bi: 0.000 to 0.010%, Nb: 0.000 to 0.020%, Al: 0.020 to 0.055%, Sn: 0.000-0.015%, V: 0.000-0.060%, B: 0.0000-0.0005%, Pb: 0.000 to 0.010%, As: 0.000 to 0.020%, Sb: 0.000 to 0.020%, Ca: 0.000 to 0.005 percent of the total weight of the alloy, the balance of Fe, and the carbon equivalent Ce less than 0.43;
B) forging, wherein the heating temperature is less than or equal to 1180 ℃, the heat preservation time is 0.5-1.5 hours/inch, the heat preservation time is not too long, and the grain size is effectively controlled; the heating temperature is less than or equal to 1180 ℃, and the temperature is not too high, so that the phenomenon that the initial forging temperature of the core part of the material is too high and the crystal boundary is melted and coarsened due to the friction heating between crystal grains in the deformation process is avoided; repeatedly upsetting and drawing the steel ingot transversely and longitudinally for three times by adopting a hydraulic press WHF forging method and a forging hammer FM forging method, wherein the single forging ratio is more than 2, the temperature in the whole forging process is controlled to be 900-1180 ℃, and the steel ingot is immediately returned to the furnace for heating when the temperature is reduced to be close to the lower limit;
C) and (3) performing heat treatment, namely normalizing at 960 ℃, quenching at 920 ℃, tempering at 610 ℃, and keeping the temperature for 1.0 hour/inch, wherein the heat treatment is calculated according to the size of the maximum wall thickness.
In a specific embodiment of the invention, the steel ingot comprises the following components in parts by weight: c: 0.08-0.10%, Si: 0.20-0.40%, Mn: 1.15-1.30%, P: 0.005-0.015%, S: 0.001-0.006%, Cr: 0.10-0.30%, Ni: 0.60-0.90%, Mo: 0.20-0.30%, Cu: 0.060 to 0.20%, Ti: 0.000 to 0.009%, Bi: 0.000 to 0.0017%, Nb: 0.000 to 0.005%, Al: 0.020 to 0.040%, Sn: 0.001-0.010%, V: 0.000 to 0.040%, B: 0.0001-0.0004%, Pb: 0.000 to 0.0015%, As: 0.001 to 0.005%, Sb: 0.000 to 0.003%, Ca: 0.000 to 0.001 percent, the balance of Fe, and the carbon equivalent Ce is less than 0.43.
In a specific embodiment of the invention, the geometric structure of the forging is considered when charging in the step C heat treatment step, and the inner hole has sufficient cooling effect during quenching; the through hole products are vertically arranged, and the blind hole products are additionally provided with a high-pressure water injection device to remove high-temperature water deposited in the blind hole products, so that the cooling effect is promoted.
The invention has the beneficial effects that: the super-large-wall-thickness (the wall thickness is more than 200mm) quick connector forge piece manufactured through component design, forging and heat treatment process optimization has excellent weldability and low-temperature performance, the problems that the design structure of deep sea oil and gas production equipment and a conveying pipeline is complex, the process is complex, the construction is difficult, the operation and maintenance cost is high and the like caused by the quick connector produced by the existing material are solved, the construction is simple, the modularization and the standardized production of the quick connector forge piece are realized, and the quick connector forge piece is used for the ultra-deep sea oil and gas production equipment and the conveying pipeline with the operating water depth of more than 1500 m.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A method for manufacturing a quick connector of an underwater oil and gas pipeline, the wall thickness of which is more than 200mm, comprises the following process steps:
A) the steel ingot comprises the following components in parts by weight: 0.08-0.10%, Si: 0.20-0.40%, Mn: 1.15-1.30%, P: 0.005-0.015%, S: 0.001-0.006%, Cr: 0.10-0.30%, Ni: 0.60-0.90%, Mo: 0.20-0.30%, Cu: 0.060 to 0.20%, Ti: 0.000 to 0.009%, Bi: 0.000 to 0.0017%, Nb: 0.000 to 0.005%, Al: 0.020 to 0.040%, Sn: 0.001-0.010%, V: 0.000 to 0.040%, B: 0.0001-0.0004%, Pb: 0.000 to 0.0015%, As: 0.001 to 0.005%, Sb: 0.000 to 0.003%, Ca: 0.000 to 0.001 percent of the total weight of the alloy, the balance of Fe, and the carbon equivalent Ce is less than 0.43;
B) forging, wherein the heating temperature is less than or equal to 1180 ℃, the heat preservation time is 0.5-1.5 hours/inch, the heat preservation time is not too long, and the grain size is effectively controlled; the heating temperature is less than or equal to 1180 ℃, and the temperature is not too high, so that the phenomenon that the initial forging temperature of the core part of the material is too high and the crystal boundary is melted and coarsened due to the friction heating between crystal grains in the deformation process is avoided; repeatedly upsetting and drawing the steel ingot transversely and longitudinally for three times by adopting a hydraulic press WHF forging method and a forging hammer FM forging method, wherein the single forging ratio is more than 2, the temperature in the whole forging process is controlled to be 900-1180 ℃, and the steel ingot is immediately returned to the furnace for heating when the temperature is reduced to be close to the lower limit;
C) and (3) performing heat treatment, namely normalizing at 960 ℃, quenching at 920 ℃, tempering at 610 ℃, and keeping the temperature for 1.0 hour/inch, wherein the heat treatment is calculated according to the size of the maximum wall thickness.
C, considering the geometric structure of the forge piece when charging in the heat treatment step, and having enough cooling effect when the inner hole is quenched; the through hole products are vertically arranged, and the blind hole products are additionally provided with a high-pressure water injection device to remove high-temperature water deposited in the blind hole products, so that the cooling effect is promoted.
The quick connector made in example 1 was subjected to mechanical testing with the following table indices:
Figure BDA0002348542560000041
note that Long represents the longitudinal direction, and Tran represents the longitudinal direction; t is the thickness of the workpiece measured in inches.
Example 2
The difference from the embodiment 1 is that the steel ingot comprises the following components in parts by weight: 0.00-0.12%, Si: 0.20-0.45%, Mn: 1.10-1.40%, P: 0.000-0.015%, S: 0.000 to 0.010 percent, Cr: 0.10-0.50%, Ni: 0.50-0.99%, Mo: 0.15-0.50%, Cu: 0.000 to 0.30%, Ti: 0.000 to 0.025%, Bi: 0.000 to 0.010%, Nb: 0.000 to 0.020%, Al: 0.020 to 0.055%, Sn: 0.000-0.015%, V: 0.000-0.060%, B: 0.0000-0.0005%, Pb: 0.000 to 0.010%, As: 0.000 to 0.020%, Sb: 0.000 to 0.020%, Ca: 0.000 to 0.005 percent, the balance of Fe, and the carbon equivalent Ce is less than 0.43.
Comparative example
When the common F65 grade material is used, the yield strength of the center position of the forge piece is lower than 450MPa under the condition of ensuring the impact performance.
After the process is adjusted to ensure that the yield strength of the central position of the forge piece reaches the requirement of 450MPa, the Charpy impact test results at the low temperature of-29 ℃ and-46 ℃ have the phenomenon that the single lowest impact value does not meet the requirement, and the deviation of three impact values of the same group is extremely large and has a difference of more than 10 times.
The above-mentioned embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be used, not restrictive; it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.

Claims (2)

1. A method for manufacturing a quick connector of an underwater oil and gas pipeline is characterized by comprising the following process steps:
A) the steel ingot comprises the following components in parts by weight: c: 0.00-0.12%, Si: 0.20-0.45%, Mn: 1.10-1.40%, P: 0.000-0.015%, S: 0.000 to 0.010 percent, Cr: 0.10-0.50%, Ni: 0.50-0.99%, Mo: 0.15-0.50%, Cu: 0.000 to 0.30%, Ti: 0.000 to 0.025%, Bi: 0.000 to 0.010%, Nb: 0.000 to 0.020%, Al: 0.020 to 0.055%, Sn: 0.000-0.015%, V: 0.000-0.060%, B: 0.0000-0.0005%, Pb: 0.000 to 0.010%, As: 0.000 to 0.020%, Sb: 0.000 to 0.020%, Ca: 0.000 to 0.005 percent of Fe and less than 0.43 percent of carbon equivalent Ce, wherein the values of Ti, Bi, Nb, Sn, V, B, Pb, As, Sb and Ca are all more than 0;
B) forging, wherein the heating temperature is less than or equal to 1180 ℃, and the heat preservation time is 0.5-1.5 hours/inch; the heating temperature is less than or equal to 1180 ℃; repeatedly upsetting and drawing the steel ingot transversely and longitudinally for three times by adopting a hydraulic press WHF forging method and a forging hammer FM forging method, wherein the single forging ratio is more than 2, the temperature in the whole forging process is controlled to be 900-1180 ℃, and the steel ingot is immediately returned to the furnace for heating when the temperature is reduced to be close to the lower limit;
C) and (3) performing heat treatment, namely normalizing at 960 ℃, quenching at 920 ℃, tempering at 610 ℃, and keeping the temperature for 1.0 hour/inch, wherein the heat treatment is calculated according to the size of the maximum wall thickness.
2. The method for manufacturing the underwater oil and gas pipeline quick connector according to claim 1, wherein the steel ingot comprises the following components in parts by weight: c: 0.08-0.10%, Si: 0.20-0.40%, Mn: 1.15-1.30%, P: 0.005-0.015%, S: 0.001-0.006%, Cr: 0.10-0.30%, Ni: 0.60-0.90%, Mo: 0.20-0.30%, Cu: 0.060 to 0.20%, Ti: 0.000 to 0.009%, Bi: 0.000 to 0.0017%, Nb: 0.000 to 0.005%, Al: 0.020 to 0.040%, Sn: 0.001-0.010%, V: 0.000 to 0.040%, B: 0.0001-0.0004%, Pb: 0.000 to 0.0015%, As: 0.001 to 0.005%, Sb: 0.000 to 0.003%, Ca: 0.000 to 0.001 percent, the balance of Fe, the carbon equivalent Ce is less than 0.43, and the values of Ti, Bi, Nb, V, Pb, Sb and Ca are all more than 0.
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