CN113466011A - Preparation method of microporous filter membrane quality control sample and quality control sample - Google Patents

Preparation method of microporous filter membrane quality control sample and quality control sample Download PDF

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Publication number
CN113466011A
CN113466011A CN202110842720.2A CN202110842720A CN113466011A CN 113466011 A CN113466011 A CN 113466011A CN 202110842720 A CN202110842720 A CN 202110842720A CN 113466011 A CN113466011 A CN 113466011A
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filter membrane
standard solution
quality control
microporous filter
control sample
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周长美
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Jiangsu Center For Disease Control And Prevention (jiangsu Institute Of Public Health)
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Jiangsu Center For Disease Control And Prevention (jiangsu Institute Of Public Health)
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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Abstract

The invention discloses a preparation method of a microporous filter membrane quality control sample and the quality control sample. The preparation method comprises the following steps: (1) selecting a microporous filter membrane; (2) preparing a standard solution; (3) subpackaging the standard solution; (4) dropwise adding a standard solution; (5) placing the microporous filter membrane added with the standard solution prepared in the step (4) in a clean tray, transferring the microporous filter membrane into an oven, and drying; (6) and (5) packaging the dried microporous filter membrane prepared in the step (5) by using an independent filter membrane box to obtain a microporous filter membrane quality control sample. The quality control sample prepared by the invention has good uniformity and stability, and can improve the accuracy and reliability of the detection work of metal poisons in the air.

Description

Preparation method of microporous filter membrane quality control sample and quality control sample
Technical Field
The invention relates to a preparation method of a quality control sample, in particular to a preparation method of a microporous filter membrane quality control sample and the quality control sample.
Background
In the aspect of metal poison detection in the air, the quality control sample has the problems of single supply party, non-uniform preparation process, few related poison types and the like for a long time. When the quality control is carried out on the detection work of metal toxicants in air, the microporous filter membrane quality control sample is prepared by adopting a labeling method. However, the differences of key links of various research and development mechanisms and laboratories such as blank microporous filter membrane selection, solution preparation and storage, microinjector selection, adding standard quantity control, microporous filter membrane packaging and the like are mastered, so that the problems of poor quality, unstable quality and the like of the currently marketed and homemade microporous filter membrane quality control samples exist, and the requirements of quality control of metal poison detection work in the air cannot be well met.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a preparation method of a microporous filter membrane quality control sample, and the quality control sample prepared by the method has good uniformity and stability, and can improve the accuracy and reliability of metal poison detection work in air. In addition, the invention also provides a quality control sample prepared by the preparation method.
The technical scheme is as follows: the preparation method of the microporous filter membrane quality control sample comprises the following steps:
(1) selection of microporous filter membrane: performing blank test inspection on the microporous filter membrane, and performing subsequent operation on the microporous filter membrane qualified in the blank test inspection; (2) preparing a standard solution; (3) subpackaging standard solution: transferring the standard solution prepared in the step (2) into a transparent jaw headspace bottle, and pressing a bottle cap of the jaw headspace bottle tightly, wherein a spacer adopted by the bottle cap of the jaw headspace bottle is a silicone rubber spacer; (4) dropwise addition of the standard solution: taking a micro-syringe, enabling a needle head to penetrate through a silicon rubber spacer to absorb the standard solution in the headspace bottle obtained in the step (3), washing the needle, discharging bubbles and absorbing the standard solution, and pulling out the needle head after the confirmation of a 'third confirmation method', injecting the needle head into the microporous filter membrane qualified by blank detection in the step (1), and ensuring that the needle head is dropwise added with the standard solution from inside to outside near the center of the microporous filter membrane; (5) placing the microporous filter membrane added with the standard solution prepared in the step (4) in a clean tray, transferring the microporous filter membrane into an oven, and drying; (6) and (5) packaging the dried microporous filter membrane prepared in the step (5) by using an independent filter membrane box to obtain a microporous filter membrane quality control sample.
Preferably, in step (1), the microporous filter membrane is required to satisfy a blank test without detection of the target compound.
Preferably, in the step (2), the standard solution is a lead nitrate standard solution, and the concentration of the lead nitrate standard solution is 1.0 mg/mL.
Preferably, the lead nitrate standard solution is prepared by the following method: accurately weighing pure lead nitrate; preparing pure nitric acid into a nitric acid solution with the concentration of 1%; dissolving lead nitrate with a small amount of nitric acid solution, transferring the lead nitrate into a volumetric flask, washing the transferred container with the nitric acid solution for multiple times, and transferring the cleaning solution into the volumetric flask to prepare a lead standard solution.
Preferably, in the step (4), the micro syringe sucks no more than 10 μ L of the standard solution.
Preferably, in step (4), the confirmation is a "three-time confirmation method": after the micro-syringe is firstly confirmed to suck a certain volume of standard solution, the volume of the micro-syringe is secondarily confirmed to be sucked without errors before the needle head is pulled out, and before the micro-syringe injects the standard solution into the microporous filter membrane, the suction volume of the micro-syringe is confirmed to be the volume of the standard solution required by the quality control sample of the batch again.
Preferably, in step (4), the injection method is: the method comprises the following steps of (1) enabling a micro-syringe needle to be close to the center of a microporous filter membrane, dripping a standard solution in a mode of drawing a spiral line from inside to outside, and slowly dripping the standard solution while moving; and in the process from inside to outside, all the absorbed standard solutions are completely dripped, and the standard solutions are ensured to be completely absorbed by the microporous filter membrane by taking the degree that no obvious liquid drops are generated in the process.
Preferably, the drying conditions are as follows: oven drying at 40-50 deg.C for 5-10 min.
Preferably, the preparation method of the invention comprises the following steps: (1) taking a qualified blank microporous filter membrane, wherein the aperture is 0.8 mu m; (2) weighing 0.1598g of lead nitrate, drying at 105 ℃ for 2h, dissolving a proper amount of nitric acid solution with the mass concentration of 1%, transferring all the lead nitrate solution into a 100mL volumetric flask, and fixing the volume to a scale which is a 1.0mg/mL lead standard solution; (3) transferring the lead standard solution prepared in the step (2) into a 15mL headspace bottle, capping and compressing, wherein the bottle cap of the headspace bottle is an aluminum cap with a spacer made of silicon rubber and polytetrafluoroethylene composite; (4) taking a 10 mu L micro-syringe, sucking 10 mu L of the lead standard solution in the headspace bottle obtained in the step (3), allowing a 10 mu L micro-syringe needle to penetrate through a silicon rubber spacer to suck the lead standard solution, washing the needle, discharging bubbles, confirming the suction amount for the second time, then pulling out the needle, and slowly dripping the needle on the microporous filter membrane in the step (1); confirming the absorption amount for the third time before dripping the lead standard solution into the microporous filter membrane; the needle head of the micro-syringe draws a spiral line outwards near the center of the microporous filter membrane, and the micro-syringe is dripped while moving, and the injection process needs to be slow; (5) drying the prepared microporous filter membrane absorbing 10 mu L of lead standard solution in a drying oven at 40 ℃, transferring the labeled microporous filter membrane into the drying oven in batches, wherein the action in the transferring process is gentle, and the overlapped or falling of the tiled labeled filter membrane is prevented; (6) and packaging the prepared and dried microporous filter membranes by using filter membrane boxes respectively, and attaching labels containing detailed information of quality control samples.
Preferably, the headspace bottle is in a 15mL transparent jaw headspace bottle specification, is matched with an aluminum cover with a 20mm spacer made of silicon rubber and polytetrafluoroethylene composite, and is pressed by a 20mm jaw headspace bottle manual capping device.
The invention also provides a quality control sample prepared by the preparation method.
Has the advantages that: the quality control sample prepared by the invention has good parallelism and high stability, the preparation method is simple and easy to popularize, and the requirement of quality control of metal poison detection in the air can be well met; has important significance for quality control in the detection process, development of the detection method and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by examples below. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention.
Example 1: a preparation method of a microporous filter membrane quality control sample, taking the preparation of a 10 mu g lead microporous filter membrane quality control sample as an example, comprises the following steps:
(1) selection of microporous filter membrane: the 15 th part of the air toxic substances in the workplace are measured by simple random non-repeated sampling of microporous filter membranes with the same batch of pore diameters of 0.8 mu m according to a measuring method GBZ/T300.15-2017: putting the filter membrane into a beaker, adding 5mL of digestive juice, covering a surface dish, slowly heating and digesting on an electric hot plate or an electric sand bath, and keeping the temperature at about 200 ℃ until the solution is colorless, transparent and nearly dry. Quantitatively transferring the residual liquid into a test tube with a plug scale by using a nitric acid solution, diluting to 5.0mL, shaking uniformly, measuring by using an atomic absorption spectrophotometer, and operating the microporous filter membrane qualified by blank test according to the subsequent steps, wherein the lead cannot be detected in the evacuated white microporous filter membrane.
(2) Firstly, putting a 10mL beaker on a balance, and zeroing; accurately weighing 0.1598g of superior pure lead nitrate; adding 10mL of superior pure nitric acid into 990mL of deionized water to prepare a nitric acid solution with the concentration of 1%; dissolving lead nitrate by using a small amount of nitric acid solution, transferring the lead nitrate into a 100mL volumetric flask, washing the beaker by using the nitric acid solution for multiple times, and transferring the beaker to the volumetric flask to ensure complete lead nitrate transfer; the volume is determined to the scale of the volumetric flask by using nitric acid solution, and 1.0mg/mL lead standard solution is prepared.
(3) And (3) transferring the lead standard solution prepared in the step (2) into a 15mL transparent jaw headspace bottle, matching with an aluminum cover with a 20mm spacer made of silicon rubber and polytetrafluoroethylene composite, and pressing by using a manual capping device of the 20mm jaw headspace bottle.
(4) Taking a 10 mu L micro-syringe, enabling a needle head to penetrate through a silicon rubber spacer to suck the lead standard solution in the headspace bottle obtained in the step (3), washing the needle, discharging bubbles, and taking 10 mu L of lead standard solution, pulling out the needle head after confirming the volume for the second time, confirming that the suction amount is 10 mu L again before dropwise adding the lead standard solution to the microporous filter membrane, then injecting the standard solution into the microporous filter membrane prepared in the step (1), ensuring that the needle head is near the center of the microporous filter membrane, dropwise adding the standard solution in a manner that the needle head draws a spiral line from inside to outside near the center of the filter membrane, and slowly dropwise adding the standard solution while moving; in the process from inside to outside, all the absorbed standard solutions are completely dripped, and the standard solution of 1.0mg/mL lead is completely absorbed by the microporous filter membrane in the injection process by the degree that no obvious liquid drop is generated in the process.
(5) Carefully placing the microporous filter membrane added with 10 mu L of lead standard solution prepared in the step (4) in a clean tray, transferring the microporous filter membrane into an oven, and drying the microporous filter membrane for 5 minutes at 40 ℃.
(6) And (5) packaging the dried microporous filter membrane prepared in the step (5) by using an independent filter membrane box, and attaching a label containing detailed information of the quality control sample.
Secondly, carrying out performance test on the quality control sample of the microporous filter membrane
2.1 sample homogeneity test
The determination method comprises the following steps: 10 pieces of the microporous filter membrane quality control sample prepared in example 1 were randomly extracted, and part 15 of the microporous filter membrane quality control sample was measured according to GBZ/T300.15-2017 workplace air noxious substance: putting the filter membrane into a beaker, adding 5mL of digestive juice, covering a surface dish, slowly heating and digesting on an electric hot plate or an electric sand bath, and keeping the temperature at about 200 ℃ until the solution is colorless, transparent and nearly dry. Quantitatively transferring the residual liquid into a test tube with a plug scale by using a nitric acid solution, diluting to 5.0mL, shaking uniformly, and measuring by using an atomic absorption spectrophotometer. The results of the uniformity test of the lead content in the microporous membrane quality control sample are shown in Table 1
TABLE 1 uniformity test results of lead content in microfiltration membrane quality control samples
Figure BDA0003179478130000041
From the inspection results in table 1, it can be seen that the relative standard deviation RSD of the lead content in the mass control samples of the microporous filtration membranes of this batch was 3.8%, which was less than 5%, indicating that there was no significant difference in the mass control samples, and the uniformity of the mass control samples of the microporous filtration membranes prepared in this batch was good.
2.2 sample stability testing
The test method comprises the following steps: and randomly extracting 6 quality control samples on the day of the preparation of the batch of quality control samples and at the 12 th month after the preparation, respectively determining the content of lead in the samples according to GBZ/T300.15-2017, taking the total average value of the 6 quality control samples as the characteristic quantity value of the time point, analyzing whether the two determination results have significant difference by adopting a T-test method, and judging the stability of the batch of prepared quality control samples. The results of the stability test and analysis of the lead content in the microporous membrane quality control samples are shown in Table 2.
TABLE 2 stability test and analysis results of lead content in microporous membrane quality control samples
Figure BDA0003179478130000051
From the stability test results in table 2, it can be seen that the test value t of the lead content in the microporous filter membrane quality control sample of the batch is 0.34 less than t (0.05,10), which indicates that the lead content in the sample has no significant difference within the experimental period of 12 months and has good stability.
If the blank test is not carried out on the blank microporous filter membrane in the improvement step (1), the background values of the microporous filter membranes with uneven commercial quality bring a plurality of uncertain factors for the preparation of the quality control sample. The invention solves the problem that the volumetric flask adopted in the prior art is filled with standard solution and the micro-syringe is inconvenient to suck by selecting the headspace bottle matched with the aluminum cover spacer in the step (3).
2.3 Effect of "triple confirmation" on quality control sample homogeneity
In the step (4), the problem that many abnormal outliers are easy to appear in the prior art is solved by adopting a micro-syringe suction volume 'three-time confirmation method', the comparison data are shown in a table 3, and quality control samples with undetected data appear.
In the step (4), 10 μ L of the lead standard solution was directly aspirated at one time, and as can be seen from table 3, the uniformity of the quality control samples obtained by one-time confirmation was significantly inferior to that of the quality control samples obtained by the "three-time confirmation method".
TABLE 3 uniformity test results of lead content in microporous filter membrane quality control samples prepared without the "three-time validation method
Figure BDA0003179478130000061
2.4 Effect of addition method of lead Standard solution on quality control sample uniformity
In the step (4), the micro-syringe needle draws a spiral line from inside to outside near the center of the microporous filter membrane while moving and slowly injecting, the method that the filter membrane cannot be absorbed by the filter membrane to form small liquid drops due to continuous dripping at one point in the industry, which is commonly used in the industry, is easy to lose and pollute is changed, the data of obviously poor uniformity caused by the continuous dripping method is shown in a table 4, and the precision is far more than 5%.
The method specifically comprises the following steps: the method for preparing the quality control samples of table 4 was the same as that of example 1 except that 10 μ L of the lead standard solution was directly injected into the needle only at the central point in step (4), and the uniformity of the prepared quality control samples was significantly lower than that of the quality control samples prepared in example 1 of the present invention.
TABLE 4 uniformity test result of lead content in microporous filter membrane quality control sample by continuous dropping method
Figure BDA0003179478130000071
As can be seen from the experimental results in Table 4, the invention increases the area of the filter membrane for absorbing the solution by slowly dripping while moving, avoids loss and pollution, and shortens the heating time of the oven.
The invention also improves the method of direct airing in the prior art, the microporous filter membrane added with the label in the step (5) of the invention is transferred into an oven, the solvent volatilization process is accelerated, the label-added filter membrane can be put into an independent filter membrane box in the shortest time, and the possibility of pollution is reduced.
In conclusion, the sample uniformity and the 12-month stability test prove that the microporous filter membrane quality control sample obtained by the preparation method has good uniformity and stability.
The above description is only exemplary of the present invention and should not be taken as limiting, any modification, equivalent replacement or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A preparation method of a microporous filter membrane quality control sample is characterized by comprising the following steps:
(1) selection of microporous filter membrane: performing blank test inspection on the microporous filter membrane, and performing subsequent operation on the microporous filter membrane qualified in the blank test inspection;
(2) preparing a standard solution;
(3) subpackaging standard solution: transferring the standard solution prepared in the step (2) into a transparent jaw headspace bottle, and pressing a bottle cap of the jaw headspace bottle tightly, wherein a spacer adopted by the bottle cap of the jaw headspace bottle is a silicone rubber spacer;
(4) dropwise addition of the standard solution: taking a micro-syringe, enabling a needle head to penetrate through a silicon rubber spacer to absorb the standard solution in the headspace bottle obtained in the step (3), washing the needle, discharging bubbles, absorbing the standard solution, pulling out the needle head after confirmation, injecting the needle head into the microporous filter membrane qualified by blank detection in the step (1), and ensuring that the needle head is dropwise added with the standard solution from inside to outside near the center of the microporous filter membrane;
(5) placing the microporous filter membrane added with the standard solution prepared in the step (4) in a clean tray, transferring the microporous filter membrane into an oven, and drying;
(6) and (5) packaging the dried microporous filter membrane prepared in the step (5) by using an independent filter membrane box to obtain a microporous filter membrane quality control sample.
2. The method as set forth in claim 1, wherein the microfiltration membrane is required to satisfy a blank test without detection of the target compound in the step (1).
3. The method for preparing a quality control sample of a microfiltration membrane according to claim 1 wherein in step (2), the standard solution is a lead nitrate standard solution, for example, for preparing a lead microfiltration membrane quality control sample, and the concentration of the lead nitrate standard solution is 1.0 mg/mL.
4. The method for preparing the quality control sample of the microfiltration membrane according to claim 3, wherein the lead nitrate standard solution is prepared by the following method: accurately weighing pure lead nitrate; preparing pure nitric acid into a nitric acid solution with the concentration of 1%; dissolving lead nitrate with a small amount of nitric acid solution, transferring the lead nitrate into a volumetric flask, washing the transferred container with the nitric acid solution for multiple times, and transferring the cleaning solution into the volumetric flask to prepare a lead standard solution.
5. The method for preparing a microfiltration membrane quality control sample according to claim 4 wherein in step (4), the standard solution drawn by the micro-syringe does not exceed 10. mu.L.
6. The method for preparing a quality control sample for a microfiltration membrane according to claim 4 wherein in step (4), the determination is a "three-time confirmation method": after the micro-syringe is firstly confirmed to suck a certain volume of standard solution, the volume of the micro-syringe is secondarily confirmed to be sucked without errors before the needle head is pulled out, and before the micro-syringe injects the standard solution into the microporous filter membrane, the suction volume of the micro-syringe is confirmed to be the volume of the standard solution required by the quality control sample of the batch again.
7. The method for preparing the microfiltration membrane quality control sample according to claim 4, wherein in the step (4), the injection method comprises the following steps: and (3) approaching the needle of the micro-syringe to the vicinity of the center of the microporous filter membrane, drawing a spiral line from inside to outside, and slowly dripping the standard solution.
8. The method for preparing the microfiltration membrane quality control sample according to claim 1, wherein the drying conditions are as follows: oven drying at 40-50 deg.C for 5-10 min.
9. A quality control sample prepared by the preparation method according to any one of claims 1 to 8.
CN202110842720.2A 2021-07-26 2021-07-26 Preparation method of microporous filter membrane quality control sample and quality control sample Pending CN113466011A (en)

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CN102247901A (en) * 2011-04-14 2011-11-23 山东电力研究院 Measuring flask used for preparation of volatile standard solution and application method thereof
AU2020102127A4 (en) * 2020-09-03 2020-10-15 Ningbo Municipal Center for Disease Control and Prevention Collection and determination of acrolein and other four aldehydes in workplace

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Application publication date: 20211001