CA1163463A - Device for pulse dosage of liquid microsamples into the flame of atom absorption spectrophotometer - Google Patents

Device for pulse dosage of liquid microsamples into the flame of atom absorption spectrophotometer

Info

Publication number
CA1163463A
CA1163463A CA000389906A CA389906A CA1163463A CA 1163463 A CA1163463 A CA 1163463A CA 000389906 A CA000389906 A CA 000389906A CA 389906 A CA389906 A CA 389906A CA 1163463 A CA1163463 A CA 1163463A
Authority
CA
Canada
Prior art keywords
distributor
sample
container
electromagnetic valve
atom absorption
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CA000389906A
Other languages
French (fr)
Inventor
Lyubomir P. Futekov
Georgi L. Bekyarov
Rina G. Parichkova
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NAUCHNO-PROIZVODSTVENO PREDPRIYATIE "B A L K A N"
Original Assignee
NAUCHNO-PROIZVODSTVENO PREDPRIYATIE "B A L K A N"
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NAUCHNO-PROIZVODSTVENO PREDPRIYATIE "B A L K A N" filed Critical NAUCHNO-PROIZVODSTVENO PREDPRIYATIE "B A L K A N"
Application granted granted Critical
Publication of CA1163463A publication Critical patent/CA1163463A/en
Expired legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/72Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/714Sample nebulisers for flame burners or plasma burners
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103Atomic absorption analysis

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  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

ABSTRACT OF THE DISCLOSURE:
A device for pulse dosage of liquid microsamples into the flame of an atom absorption spectrophotometer, including a distributor and an electromagnetic valve, characterized that the device is constructed of two units at most, the units being located at different levels in respect to the pulverizer of the atom absorption spectro-photometer, wherein the distributors are of the three-way type and there is a connection provided between the distributors and the electromagnetic valves, the three-way distributor of the higher level unit being connected to a container for the sample, to the atmosphere by means of an electromagnetic valve and to the pulverizer of the atom absorption spectrophotometer by means of the three-way distributor of the lower level unit, said distributor of the lower level unit being connected to a container for the sample solvent.

Description

The present invention relates to a de~ice for pulse dosage of liquid microsamples into the flame oE an atom absorption spectrophotometer ~A~S).
Device for puIse dosage of liquid microsamples into the flame of AAS are known, whlch consist in a polytetra-fluoroethylene funnel which is connected to the aggregate for spraying of the sample by means of a special capillary. The dosage of the solution in a volume of 50-100 microliters is performed manually, using microllter pipettes provided with special movable plastic nizzles (1).
It is known also a device for automatic pulse dosage of liquid microsamples into the flame of AAS, which is constructed based on the studies performed by Berndt and Jackwerth (2) and used by " Perkin Elmer" . It consists a combination of Teflon funnel provided with a microliter ~ . . .
pipette and a small pump, a system for circular step moving of a table, where beakers containing samples to be tested are laid upon. The operation of the device depends on the electronics of the atom absorption spectrophotometer. It 20 permits an automatic dosage of samples of volumes 50 or 100 microliters.
A manual-acting device for pulse dosage is known, which consists in a small container of conical bottom. The sample of a preliminary known volume of 50-500 microliters is pumped only once by the capillary, said capillary being connected to the pulverizer of the AAS(3).
It is a common disadvantage of the well known automatic devices tha-t these are extremely expensive~
In manual-acting devices for pulse dosage, relatively high cost microli-ter pipettes o~ movable nozzles are used and the dosage is both unconvenient and tiresome when lar~e number of samples are to be tested, which xesults in a lower reproducability.
The ~bject of the presen~ invention is to provide a device for pulse dosage of liquId microsamples into the flame of atom absorption spectrophotometer, said device being such as to enable a simple, fast, reliable, precise and convenient handling of the samples at bo-th a good reproduc-ability and low cost.
This object is achieved by a device for pulse dosage of li~uid microsamples into the flame of an atom absorption spectrophotometer, including a distributor and an electromagnetic valve, characterized in that the device is constructed of two units at most, the units being located at different levels in respect to the pulverizer of the atom absorption spectrophotometer, wherein the distri~utors are of the three-way type and there is a connection provided between said distributors and the electromagnetic valves, the three-way distributor of the higher level unit being connected to a container for the sample, to the atmosphere by means of an electromagnetic valve ana to the pulverizer o the atom absorption spectrophotometer by means of the three-way distrib-utor of the lower level unit, said distributor of the lower level unit being connected to a container for the sample solvent.
Preferably, only one unit is used, where its electromagnetic valve is connected to the atmosphere and its three-way distributor is connected directly to the pulverizer of the atom absorption spectrophotometer.
In a further embodiment where still only one unit is used, its electromagnetic valve may be connected to a container for the sample solvent and its three-way distributor maybe connected directly to the container for the sample under test.

Each of the three-way distributors may be provided i3 with a cna~nel, which connects it with the electromagnetic valve, s~id channel bein~ connected to a -through-hole, wherein an angle o~ between 15 and 165 is concluded between said channel and said through-hole. The -through-hole can be oE a constant as well as step variable cross section.
The device according to the invention possesses the following advantages: there is no need for microliter pipettes; dosed volumes can be smoothly variated starting from 50microliters to a continuous pulverization; the device is universal-purpose concerning its applicability; a pos-sibility is created one to work in a mode of lntegration of the signals at a minimal volume zeroing in the flame according to the respective solvent used, followed by a pulse dosage of a microsample in the same solvent; a continuous dosage of the solvent and pulse dosage of the sample, thereby maintaining the flame stoichometry and ensuring a simplicity, conveniency, reliability, fastness and exactness in opexation.
Moreover, the device is readily available and low cost.
~mbodiments of the invention are shown as examples without limitative manner in the accompanying drawings, where:
Fig. 1 is a diagram of the device for pulse dosage of liquid microsamples into the flame o~ AAS;
Fig. 2 is a further diagram of a device for pulse dosage of liquid unicrosamples into the rame of AAS, Fig. 3 is a diagram of a further embodiment of the device, consisting of a single unit.
Figure 1 consists in two units located ak different levels over the AAS pulveraizer, where three-way distributors connected to electromagnetic valves are used. The three-way distributor 1 of the higher level unit is connected to a container for the sample by means o~ an opening 21 at the through hole 2 as well as to the atmosphere by means of an 39L~j3 electromagnetic valve 6 through -the channel 31 and opening 22 at the through-hole 2, usin~ the cube 4 provided with the opening 23 at the through-hole 20 of the three-way distributor 10 pertaining to the lower level unit, said three-way dis-tributor 10 being connected both to a container 5 for the sample solvent by means of the lower level unit electromagnetic valve 60 through the channel 32 and to the pulverizer of the AAS by means of the opening 24 at the through-hole 20.
There is an angle of 90 concluded between the through-holes 2 and 20 in the three-way distributors 1 and 10 and the channels 31 and 32 provided for connection with the corresponding electromagnetic valves.
' The device operates as follows: The flame of the AAS is ignited. Both electromagnetic valves 6 and 60 are opened. The pure solvent contained in the container 7?passes through the electromagnetic valve 60, channel 32, opening 24 and by means of a plastic tube enters the pulverizer (or, respectively, flame of the AAS). A portion of the solvent is ascended along the plastic tube 4, thereby forming a hydraulic seal against the air inlet from the electromagnetic valve 6.
No suction of solution of the liquid sample occurs. Thus, zeroing of the apparatus takes place under said conditions.
A higher rate of solvent admission is ensured compared with the liquid consumption of the pulverizer due to the higher level of the container 5 compared with the level of the pulverizer and by the proper choice of the cross sections of channels 32 and 2.
The two electromagnetic valves 6 and 60 are closed during a short strictly defined time by means of electro-magnetic releys actuated by a signal, submit-ted by the operator.

~L~63~

The dosage of pure solvent stops in the manner described ~bove. `The liquid sample is pumped and enters the AAS
pulverizer through a plastic tube after being passed through a plastic ~ube, the opening 21, the through-hole 2, the opening 22, the plastic tube ~, the opening 23, the through-hole 20 and opening 24. Pulverization of the pure solvent is restored after the opening of the electromagnetic valves 6 and 60. The amount of volumes being dosed is controlled by the duration of the closure time of the electromagnetic valves.
The device permits a continuous dosage of the solvent and pulse dosage of the sample, i.e. sample-solvent-sample... without any air feeding, which results in an improvement of the flame parameters or, respectively, efficiency of the atomization of a number of elements, while ensuring the possibility one to work without deuterium correction.
Results obtained using the above outlines device are given in Table 1.
The embodiment of Figure 2 is constructed of a single unit. The three-way distributor 1 of said unit contacts with the atmosphere by means of a channel 31 and electro-magnetic valve 6; with the container for sample under test by means of the opening 21 at the through-hole 2 and directly with the pulverizer of AAS by means of the opening 22 at the through-hole 2.
This device operates as folIows. The opening 22 is connected to the pulverizer of AAS by means of a plastic tube.
Then, the control panel of the electromagnetic valve 6 is switched on to the electric set. The flame of AAS is ignited.
Zeroing of the apparatus can be made either on the flame or corresponding solvent used.

A signal submitted by the operator closes the ~;39~63~

electromagnetic valve Eor a short strictly de~ined time, said time being controlled by electronic timers. The air access to the through-hole 2, comming from the electromagnetic valve 6 through the channel 31, is disconnected. The solution of the samplc under test is pumped for a short time and passes through: a plastic tube, the opening 21, the through-hole 2, the opening 22 and then, by means of a plastic tube enters the pulverizer of AAS. Thus, pulse dosage of liquid micro-samples is accomplished, which stops at the moment of opening of the electromagnetic valve 6, i.e. a dosage of the type sample-air sample...is performed. The amount of the volumes being dosed is determined by the closure time of the electro-magnetic valve 6.
Results obtained using the above said device are given in Table 2.
The embodiment of Figure 3, the device consists in a single unit. The three-way distributor 10 of said unit is connected to a container 5 for the sample solvent, to the electromagnetic valve 60 and channel 32, to a container for the sample under test by means of the opening 23 at the through-hole 20 and to the pulverizer of AAS by means of the opening 24 at the. same through-hole 20.
In all possible versions of embodiment of the device, the through-holes 2 and 20 can be of either constant (Figs. 1,2) or step variable (Fig.3) cross sections.

Relative absorption from 15 measurements performed over solutions in the flame of AAS after a pulse dosage of the type sample-solvent-sample...using the device according to the invention.

ELEMENT CONCENTRATION SOLVENT A SR

-mkg-ml 1 Cu 2,0 MMK 0,147 5,32 10,0 H2O0,197 2,26 0,4 MMK0,141 2,24 Cd 4,0 ~2 0,298 3,32 Te 4,0 MMK0,2Z4 6,29 __ 10,0 MMK0,518 0,70 Pb 10,0 H2O0,095 5,20 4,0 MMK0,284 1j42 Fe 4,0 H2O0,042 6,47 _ 50,0 - xylene 0,280 Al 50,0 H2O0,300 50,0 MIBK0,790 Sn 50,0 ~120,120 Organic solutions of Cu, Cd, Te and Pb are obtained by extraction of the diethyldithiocarbamate complexes of Cu, Cd, Te and Pb with methylmetacrylate. The Fe is extracted as a hydrochloric acid complex, and the Sn and Al are extracted as standard caproate solutions MMK = methylmetacrylate MIBK = methyiisobutyl ketone Absorption o~ solutions in the ~lame of AAS, measured after pulse dosage of the type sample-air-sample...

DEVICE ~CCORDING324,7nm -228,8nm ma~~217,Onm TO THE INVENTIONsplit-0,7 1split-0,7 1 split-0,7 Cu-1,5mkg ml Cd-0,4mkgml Pb-S,Omkg.ml A` SR % A SR % A SR %
aqueous device0,065 1,580,032 7.08 0,093 1,65 solutions funnel P.E. 0,058 4,33 0,027 9,48 0~074 4r88 _ solutions device0,253 0l660,127 2,82 0,076 4,60 .
MIBK Funnel P.E.0,256 0,860,100 3,28 0,081 5,04 solutions device0,221 1,180,107 3,53 0,061 5,67 .
MMK Funnel P.E.0,220 1,180,105 3,68 0,062 7,50 solutions device0,118 1,730,084 7,88 - -0,108 0,91 __ TOLUENE Funnel P.E. 0,126 1.92 0,048 7,68 .
Absorption values are average of 25 measurements (II).
x zeroing performed on organic solvent. In other cases, zeroing is accomplished based on the flame.
MIBK = methylisobutyl ketone MMK = methylmetacrylate SR ~ = relative standard shift

Claims (6)

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:
1. A device for pulse dosage of liquid microsamples into the flame of an atom absorption spectrophotometer, including a distributor and an electromagnetic valve, characterized in that said device is constructed of two units at most, said units being located at different levels in respect to the pulverizer of the atom absorption spectro-photometer, wherein the distributors are of the three-way type and there is a connection provided between said distributors and the electromagnetic valves,the three-way distributor of the higher level unit being connected to a container for the sample, to the atmosphere by means of an electromagnetic valve and to the pulverizer of the atom absorption spectrophotometer by means of the three-way distributor of the lower level unit, said distributor of the lower level unit being connected to a container for the sample solvent.
2. A device according to Claim 1, characterized in that when a single unit is used, where the electromagnetic valve of said unit is connected to the atmosphere, the three-way distributor is connected directly to the pulverizer of the atom absorption spectrophotometer.
3. A device according to Claim 1, characterized in that when a single unit is used, where the electromagnetic valve of said unit is connected to a container for the sample solvent, the three-way distributor is connected directly to the container for the sample.
4. A device according to Claim 1, characterized in that each of the three-way distributors is provided with a channel connecting said distributors with the electromagnetic valves, said channel being connected to a through-hole, wherein an angle of from 15° up to 165° is concluded between said two channels.
5. A device according to Claim 4, characterized in that the through hole is of a constant cross section.
6. A device according to Claim 4, characterized in that the through hole is of a stepwise variable cross section.
CA000389906A 1980-11-12 1981-11-12 Device for pulse dosage of liquid microsamples into the flame of atom absorption spectrophotometer Expired CA1163463A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BG49640 1980-11-12
BG8049640A BG33390A1 (en) 1980-11-12 1980-11-12 Apparatus for impulse dosing of liquid microsamples in atomicabsorbing spectrophotometer flame

Publications (1)

Publication Number Publication Date
CA1163463A true CA1163463A (en) 1984-03-13

Family

ID=3908178

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000389906A Expired CA1163463A (en) 1980-11-12 1981-11-12 Device for pulse dosage of liquid microsamples into the flame of atom absorption spectrophotometer

Country Status (8)

Country Link
JP (1) JPS57149948A (en)
AT (1) AT389766B (en)
BG (1) BG33390A1 (en)
CA (1) CA1163463A (en)
DE (1) DE3144997C2 (en)
FR (1) FR2493988A1 (en)
GB (1) GB2088054B (en)
SU (1) SU1219959A1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3818058A1 (en) * 1988-05-27 1989-12-07 Bodenseewerk Perkin Elmer Co DEVICE FOR SUPPLYING LIQUID TO A SPRAYER IN A SPECTROMETER
JPH0462658U (en) * 1990-10-04 1992-05-28

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1673348A1 (en) * 1966-10-20 1972-01-13 Zeiss Carl Fa Method and device for the spectroscopic analysis of solids, solutions and gases
DE1815958B1 (en) * 1968-12-20 1970-06-18 Zeiss Carl Fa Device for the modulated supply of a sample liquid to a spectroscopic light source, e.g. a flame
GB1304883A (en) * 1969-05-13 1973-01-31
FR2181225A5 (en) * 1972-04-18 1973-11-30 Erap Elf Entr Rech Activ Petro
DE2519826A1 (en) * 1975-05-03 1976-11-04 Der Bundesminister Fuer Forsch Metering small liquid sample - by injection with gas contg. water droplets to flush out sample
US4208372A (en) * 1977-04-26 1980-06-17 Bodenseewerk Perkin-Elmer & Co., Gmbh Apparatus for generating and transferring a gaseous test sample to an atomic absorption spectrometer
DE2805137C2 (en) * 1978-02-07 1984-10-04 Bodenseewerk Perkin-Elmer & Co GmbH, 7770 Überlingen Device for automatically feeding liquid samples to a burner of a flame atomic absorption spectrometer

Also Published As

Publication number Publication date
DE3144997A1 (en) 1982-07-29
FR2493988A1 (en) 1982-05-14
JPS57149948A (en) 1982-09-16
SU1219959A1 (en) 1986-03-23
BG33390A1 (en) 1983-02-15
DE3144997C2 (en) 1985-03-28
ATA478181A (en) 1989-06-15
AT389766B (en) 1990-01-25
JPH0158452B2 (en) 1989-12-12
GB2088054B (en) 1985-01-16
GB2088054A (en) 1982-06-03
FR2493988B1 (en) 1984-11-23

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