JPS60197211A - Pretreatment apparatus - Google Patents

Abstract

PURPOSE:To supply a specimen solution containing no solid substance to an analytical apparatus, by separating a solid substance containing microbial cells in a fermented solution from the specimen solution by utilizing such a phenomenon that microbial cells are adsorbed by floc of iron hydroxide formed by adding iron chloride to the fermented solution. CONSTITUTION:The specimen solution 9 containing microbial cells from a fermented solution tank 8, the iron chloride solution 21 from an iron chloride storage tank 11 and the caustic soda solution from a caustic soda storage tank 12 are respectively supplied to the mixing tank 2 of a flocculative treatment tank 1 at every definite amount and, at the same time, a stirrer 6 is rotated by a magnetic stirrer 7 to stirr the specimen solution. The pH of the specimen solution 20 is adjusted to 7.0 or more by this operation to form floc 5 of iron hydroxide and the microbial cells in the specimen solution are adsorbed by said floc 5. Next, the specimen solution 20 containing the floc 5 is flowed to a stay tank 3 from a transfer port 4 and, thereafter, continuously supplied to a continuous centrifugal separator 16 in a definite amount to be separated into floc 18 of iron hydroxide and a supernatant solution 17 and the supernatant solution 17 is sent to liquid chromatography while the floc 18 is stored in a floc receiving tank 19.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Application of the Invention] The present invention relates to a solid-liquid separation device for fermentation liquor, and more particularly to a pretreatment device for an analytical device such as a liquid chromatograph.

[Background of the invention]

Conventionally, centrifuges and filters have been used to separate the solid matter containing bacteria in the fermentation liquid, but centrifugation makes it difficult to separate bacteria that have a specific gravity that is not much different from the sample liquid. However, in the case of filter filtration, the filter becomes clogged quickly, and samples cannot be continuously analyzed.

[Purpose of the invention]

An object of the present invention is to provide a pretreatment device that can separate solid substances, including bacterial cells, etc. in a fermentation liquid from a sample liquid, and supply a sample liquid free of solid substances to an analysis device such as a liquid chromatograph. It's about doing.

[Summary of the invention]

If the sample liquid contains solids, it is necessary to perform pretreatment for solid-liquid separation before introducing the sample liquid into an analytical instrument (liquid chromatograph, atomic absorption 9, etc.), and the simplest method is , there is a filter filtration method. However, with this method, the filter quickly becomes clogged and must be replaced frequently, making continuous sample analysis very difficult. Continuous centrifugation is a great way to pre-process samples, but it is extremely difficult to separate substances such as bacterial cells, which have a low specific gravity and have a significant difference in specific gravity from the sample solution. be. Therefore, in the present invention, in order to improve these points, iron chloride is added to the fermentation liquid at a concentration of about 1 to 209/l, and the pH is adjusted to 7.0 or higher, so that bacterial cells etc. are adsorbed to the produced iron hydroxide flocs. By focusing on this, we adsorbed microbial cells, etc. to iron hydroxide flocs, increasing their specific gravity, and processing them in a continuous centrifuge (rotation speed:
11,000 rp or higher) This is a pretreatment device characterized by separating and removing fine particles such as bacterial cells from a sample liquid.

[Embodiments of the invention]

Examples of the present invention are shown below.

The configuration and operation of the present invention will be explained with reference to FIGS. 1 and 2. The sample liquid 9 containing bacterial cells etc. is transferred from the fermentation liquid 4I118 to the mixing tank 2 of the flocculation treatment tank 1 by the sample liquid transfer metering pump 10.
is supplied in fixed amounts to

At the same time, a metering pump 13 for supplying iron chloride from the iron chloride storage tank 11
The iron chloride solution 21 is supplied to the mixing tank 2 in a fixed amount at a time, and similarly, the caustic soda solution 22 is supplied from the caustic soda storage tank 12 to the mixing tank 2 by the caustic soda supply metering pump 14.
supplied to At the same time that the sample liquid 20 is supplied into the mixing tank 2, the stirrer 6 is rotated by the magnetic stirrer 7 to stir the sample liquid 20. With this operation, the sample liquid 20
PH becomes 7.0 or higher, iron hydroxide flocs 5 are generated, and bacterial cells and the like in the sample solution are adsorbed to the flocs 5.

Next, the sample liquid 20 containing the flocs 5 flows from the transfer port 4 at the bottom of the mixing tank 2 to the retention tank 3, and from there is continuously supplied in a fixed amount to a continuous centrifuge 16 by a centrifugal metering pump 15. The hydroxylated flocs 18 adsorbing solid matter such as bacterial cells are separated into a supernatant liquid 17, and the supernatant liquid 17 is stored in a liquid chromatograph, and the flocs 18 are stored in a floc receiving tank 19. The above operations are performed continuously to continuously analyze the main components in the fermentation liquid.

Next, the results of experiments conducted using actual samples will be explained. The configuration and operation are the same as described above.

1. Experimental conditions ■) Sample liquid: Amino acid fermentation liquid (medium: bouillon medium) (Bacteria cell number ClXl0 value) l) Sample liquid supply amount: 10 d/piece 1 l) FeCAa supply amount (10% solution)・1mJ
/m (concentration in mixing tank 10g/l') IV) NaOH supply amount (10% solution') ・1 mA
/M (PH in the mixing tank: 9.0) ■) Centrifugation-like supply amount...12 d/mvl) Centrifuge rotation speed...3000 rpmvn) Coagulation treatment tank molten volume...Mixing tank: 50 m1 retention Tank: 5QIILe Total: ioom 2, Experimental results - As a result of measuring the number of bacterial cells in the supernatant after centrifugation, 10-
100 pieces/11 Ll, and no clogging of the piping was observed during amino acid measurement using liquid chromatography.

(Effects of the Invention) According to the present invention, it is possible to continuously separate and remove solids from a fermentation liquid containing bacterial cells, etc., which is very effective in automatically managing the fermentation liquid.

[Brief explanation of the drawing]

FIG. 1 is a route diagram of a sample liquid and a pretreatment device consisting of an aggregation treatment tank and a continuous centrifugal separator, and FIG. 2 is a plan view of the aggregation treatment tank viewed from above. 1... Coagulation treatment 41 #2... Mixing tank 3... Retention tank 5... Iron hydroxide floc containing bacterial cells 16... Continuous centrifugal separator 17... Supernatant liquid agent J Genshi Akio Takahashi

Claims (1)

[Claims] 1. A coagulation treatment tank consisting of a mixing tank for stirring the microbial cells, etc. in the sample solution, a retention tank for detonating, a rotor, and a magnetic stirrer, and a An iron chloride storage tank for storing the iron chloride solution and the caustic soda solution to be added to the mixing tank, a caustic soda storage tank, and a transfer pump for transferring the chemical solution to the stirring tank; A pretreatment device comprising a continuous centrifuge that separates flocs and sample liquid.