an article on CO2 gas analytic methods prior to 1958

1
Direct chemical determination of local effective CO2 concentration prior
to 1958; history and evolution of methods
@Ernst-Georg Beck, Dipl. Biol. 2006-2009
extract from: History of gas analysis, unpublished manuscript 2009
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2.2 Methods
Prior to the selective measurement procedures adopted by Keeling on the Mauna Loa volcano in
1958, all atmospheric CO2 measurement was conducted as direct local effective determination of a
distinct amount of air using chemical methods and were mostly inclusive of CO2 dissolved in humidity.
Figure 2-2.
Methods of chemical CO2 gas analysis
Nearly all known procedures to determine CO2 in air by chemical means insist on the principles
presented in Figure 2-29: i.e.
1.Accessing a fixed volume of air in a container called an “Aspirator”
2.Absorption of this volume in a strong alkaline solution
3.Determination of the absorbed amount of CO2 by analysis of the generated reaction product or
the induced change of state of absorbing solution generated by the chemical reaction
Step 3 can be done by weighing (gravimetric) or titrating (titrimetric) the carbonate as the reaction
product or by determination of changes in volume, pressure, pH or conductance of absorbing alkaline
solution.
1
2
Gravimetric methods were widely used early in the 19th century but were replaced by titrimetric
methods around 1850. In the early 20th century these methods were also replaced by volumetric and
then manometric methods.
2.2.1 Selected scientists and their developments
Qualitative and quantitative gas analysis of air started in 18th century. It
was first conducted in 1770 by Lavoisier, Priestley, Scheele, Cavendish,
Humboldt, Dalton, de Marti, Gay-Lussac, de Fontanelle, Volta, Henry and
de Saussure [Benedict 1912, Lundegardh 1924, Letts et al. 1902,
Effenberger 1951].
In 1772 Priestley and in 1778 Scheele each
discovered that air consists of several parts but with approx. one fifth
oxygen and the rest mostly nitrogen. Priestley designed the nitrogen
Eudiometer [Beretta 2007], which was then used for decades to measure
the oxygen content of air. Several variants of this device were used in
Europe by many scientists including Lavoisier and Humboldt. A sample of
air was burned in a glass vessel with NOx – later H2 – to determine the
oxygen concentration in the sample.
The Eudiometer designed by Cavendish consisted of a glass vessel
closed at its top and containing 2 electrodes for generating an electrical
spark. The bottom of the vessel was immersed in water. Air volume in
Eudiometer was noted. A known volume of H2 was added and the mixture
was ignited by a spark. The remaining volume of gas was used to
determine the oxygen that had been consumed by the combustion.
Figure 2-3.
The Eudiometer used by Henry Cavendish (1731-1810);
Patrick's College in Maynooth, County Kildare, Ireland.
http://physics.kenyon.edu/EarlyApparatus/Thermodynamics/
Eudiometer/Eudiometer.html
In 1832 Volta developed an improved Eudiometer that achieved a remarkable accuracy of 0.2% as
indicated by the difference between similar samples. Earlier measurements already existed. From
1804 De Saussure used a type of Eudiometer to measure atmospheric oxygen and CO2 contents
near a lake in Geneva. He obtained results of an average of 21.05% for oxygen and as a difference
0.04% for CO2, and prior to that at the end of the 18th century his father had been measuring
atmospheric CO2 content in the Swiss Alps by absorbing in lime water.
NICOLAS THÉODORE DE SAUSSURE, (1767 –1845) [60, B1]
Swiss chemist and plant physiologist worked in Geneva (Switzerland)
and neighbourhood.
Founder of modern plant physiology
Later on his son, Theodore, used baryta water (Ba(OH)2) and determined the produced amount of
BaCO3 by weighing to determine atmospheric CO2 content. For example, in 1829 he measured the
atmospheric CO2 content to be 0.0385% = 385 ppmv [Benedict 1912, Letts et al. 1902]. These
gravimetric methods were also used by other scientists (e.g. Thenard, Brunner, Boussingault; [Letts et
al. 1902]) in several variants up to the middle of the 19th century.
2
3
Especially the French school of gas analysts often received erroneous results because they had a
practice of drying air samples using H2SO4 with resulting absorption losses of CO2. Also, weighing
errors, absorption losses by long connections and natural rubber were pointed out by Hlasiwetz 1856
[Hlasiwetz 1856], Spring 1886 [Spring et al. 1885], Letts and Blake 1898 [Letts et al. 1902], Warburg
1909 [Warburg 1909] and Martin et al. 1933 [Martin et al. 1933].
A landmark in gas analysis was established by the German physician Max v. Pettenkofer in 1858 (the
founder of modern hygiene) when he developed a titrimetric method [Pettenkofer 1862] named in
honour of him the “Pettenkofer Process”.
A theoretical accuracy of ± 0.0006 % was provided by the Pettenkofer Process, in practice an
accuracy of practical ± 2% compared to the measured value [Pettenkofer 1866, Kauko et al. 1935,
Gorup 1866] could be achieved. Pettenkofer constructed a respiration apparatus for measuring gas
exchange by man and animals up to an accuracy of 0.1 mg. (For comparison: 1 Litre of air contains at
the moment 380 ppm CO2 = 0,038 Vol% = 0, 38 ml CO2 with a mass of 0.75 mg)
Using this method Pettenkofer and Voit established scientific base for nutrition science by resolving
balances of C-,O- and N.
MAX v. PETTENKOFER (1818-1901) [B2]
Physician at Munich,
Founder of modern Hygiene
Pettenkofer Process and Pettenkofer Number named in honour of
him
Up to 1960 the Pettenkofer Process was standard in gas analysis in its several variants because of
its easy, fast and accurate handling. [Pettenkofer 1862, 1866, Hart 1930, Klemme 2003, Gorup 1866]
This titrimetric method was based on the absorption of the CO2 from air in baryta water and titration
of the produced barium carbonate with acid. Table 0 summarises the used variants of the method:
Since 1860 innumerable scientists determined gas exchange of plants, animals and CO2 content of
air. Plant physiologist Henrik Lundegardh (1888-1969) measured the atmospheric CO2 concentration
in southern Sweden with an accuracy of ±-0.0003 volume% ( = +-1% compared to 300 ppm) between
1920 and 1926 [Lundegardh 1922]. Up to 1950 many long time sampling series existed and were
extensively tested against other methods.
Table 1.
Long time series of atmospheric CO2 concentration obtained since 1855 using the
Pettenkofer Process (double to quadrouple determinations not counted):
year
name
location
Number of
measurements
1.
2.
3..
4.
5.
6.
since 1855
1856 (6 month)1
1863 -1864
1864/65
1868 - 1871
1872 – 1873
v. Pettenkofer
v. Gilm1
Schulze
Smith
Schulze *
Reiset
Not researchable
7.
8.
9.
10.
1873
1874 –1875
1874 -1875
1877 -1910
60
295
347
12000
11.
12.
13.
14.
15.
1879 - 1880
1883
1886 - 1887
1887 -1889
1889 - 1891
Truchot
Farsky *
Hässelbarth*
Levy/ Marie-Davy;
Montsouris Observatory
Paris
Reiset
Spring
Uffelmann
Feldt, Heimann, v.Frey
Petermann
Munich (Germany)
Innsbruck1 (Austria)
Rostock, Baltic Sea (Germany)
London, Manchester, Scotland
Rostok, (Gemany)
Dieppe, France (North Sea)
(France
Clermont Ferrand (France)
Tabor, Bohemia, (Czech R.)
Dahme (Germany
1877-1910; (France)
Dieppe (France)
Liege (Belgium)
Rostock (Germany)
Dorpat (=Tartu, Estonia)
Gembloux (Belgium)
118
266
420
1534
525
19
426
246
1600
92
3
4
16.
17.
18.
19.
20.
1897 - 1898
1898 - 1901
1917 -1918
1920-1926
1925 -1927
Letts&Blake
Brown& Escombe
A. Krogh
Lundegardh, H.
Wattenberg, H.
near Belfast (Ireland)
Kew Garden England (GB)
Kopenhagen (Danmark)
Southern Sweden (Kattegat)
Tropical and southern Atlantic
Oean
Kopenhagen (Danmark)
Northern Atlantic/Finland (Finland)
near Bern (Switzerland)
Poona, India (India)
Hamburg (Germany)
Ames (IOWA, USA)
Vienna (Austria
Scandinavia
64
92
Not researchable
>3000
>9000
Not researchable
Krogh/Rehberg
Buch
176
Duerst
>1000
Misra
> 250
Effenberger
>40
Chapman et al.
>100
Steinhauser
>500
Fonselius et al.
>3400
Bischof
1
v. Gilm: Titration after drying, solving in HCl for Chlorus destination.
*
identical variant of Pettenkofer method, air sample was conducted by tube in the window of the
laboratory
21.
22.
23.
24.
25.
26.
27.
28.
1928
1932 -1935
1936 - 1939
1941 -1943
1950
1954
1957
1955-1960
Henri Victor Regnault 1810 – 1878 [B3]
Famous French chemist and physicist,
discovered carbon tetrachloride, vinyl chloride
Jules Reiset [B4]
French chemist
Basic work on animal respiration (Regnault et al.
1849)
Regnault and Reiset also investigated gas exchange in animals and 10 years earlier than Pettenkofer
[Cheng 1992]. They used Regnaults volumetric gas analyzer. Reiset himself analysed CO2 in air
using mobile modified Pettenkofer equipment [Reiset 1979] from 1872 until 1879 at his station near
Dieppe (Normandy, France, North Sea).
August Krogh (1874 –1949) [B5]
Danish physician an zoologist, Nobel award 1920
Pionieer in blood gas metabolism [Krogh 1906,1920,
1929])
Otto Warburg (1883-1970) [B6]
German chemist, Nobel award 1931 in medicine
[Warburg 1909]
Nobel laureates August Krogh (Nobel award 1920 in medicine) and Otto Warburg (Nobel award in
physiology 1931) developed improved gas analysers according to Pettenkofer achieving an accuracy
down to 0,0003 Vol% (Lundegardh 1920, [Lundegardh 1922]).
Pettenkofer variants were used for gas analysis in air and liquids until 1960; e.g. Lundegardh (192026) [Lundegardh 1922, 1924], Wattenberg 1925-27 [Wattenberg1933], Buch (1933-36) [Buch 1948],
Duerst (1936-38 [Duerst 1939]), Steinhauser 1957/58 [Steinhauser 1958] or Bischof (1955-1960)
[Bischof 1960].
4
5
Henrik Lundegardh (1888 -1969 ) [100, B7]
Swedish botanist, pioneer in plant physiology
[Lundegardh 1922, 1924, 1949]
At the end of the 19th century the first gasometric analysers were developed which work either by
volumetric [Martin 1933] or later manometric determination of gas contents. In some cases water
was absorbed before gas analysing.
Müntz und Aubin [Müntz et al. 1982] analysed the CO2 content of air at different localities in France
(Paris, Pyrenees).
Table 2.
Volumetric / manometric measurements
year
name
1
2
1875 (March)
1880 - 1882
Tissandier [222]
Müntz & Aubin [71]
3
4
1910 - 1912
1920 -1930
Benedict [51]
Rheinau [156]
5
6
7
8
9
10
11
12
13
1925-1927
1932 -1970
1912 -1936
1934
1939-1941
1940
Summer 1941
1941
1946-1961
Wattenberg [283]
v. Slyke [87]
Haldane [84,192]
Waugh
Kreutz [91]
Bazett [85]
Fuller [285]
Lockhart et al. [116]
Scholander [96, 97]
Location and
(analyzer type)
Paris, Balloon (volumetric)
near Paris, Pyrenees,
Caribbean etc. /F) volumetric
Washington (USA), volumetric
Germany, Davos, Switzerland
(Petterson/Sonden)
Atlantic Ocean; Haldane
Worldwide manometric
Worldwide volumetric
USA Haldane variant
Germany volumetric
USA, Haldane
USA, Haldane manometric
Antarctica, Haldane
Worldwide volumetric
Number of
measurements
<10
81+
>264
>500
>1000
many
1500
64 000+
>12
144
> 37
>1000
Volumetric gas analysers prior to Haldane [Haldane 1912] and Benedict/Sonden/Petterson (approx.
1900, [Benedict 1912, Petterson 1895, Sonden 1895]) were open systems without efficient control of
temperature (change of temperature gas with 1° = vol/pressure change by 0.34%; [Schuftan 1933])
and heat of absorption (approx. 20 000 cal/gMol; [Schuftan 1933]). All measuring pipettes were in a
well tempered water bath in Haldane's and Pettersons' analysers.
Therefore, earlier measurements using open systems were in considerable error (see Muentz&Aubin)
J.S. Haldane (1860 - 1936 ) [B8]
British physiologist, pioneer of compression technology and oxygen
therapy [Haldane 1912]
5
6
Francis Gano Benedict, 1870-1957 [B9]
US chemist, founder of sports medicine; pioneer of nutrition science;
investigated energy metabolism [Benedict 1912, Maynard 2004]
Air gas analysers designed by Haldane and Benedict/Sonden/Petterson are among the most
successful in the history of medicine. They were used up to 1960 for precise measurement of blood
gas levels. Still today people use the Harris-Benedict-formula for calculating BMR (Basal metabolic
rate), and this formula was developed with the help of the famous gas analyser of
Petterson/Benedict/Sonden.
In 1924 Donald D. van Slyke (a pioneer in protein and acid metabolism, blood gas analysis) designed
the first manometric gas analyser. [van Slyke 1932, NAS 1976]. In principle CO2 is absorbed out of an
air stream by NaOH with liberation of HCl and the amount of CO2 is determined by pressure change.
This equipment was used in blood gas analysis as standard for 50 years [West 2004].
Donald Dexter van Slyke 1883 –1971, [B10]
Chemist , New York,
Pioneer in blood gas measurement and protein metabolism
Until the 1930s many modified versions of the gas analysers by Pettenkofer, Haldane and
Petterson/Sonden were developed including colorimetric and pH-metric methods.
During the 30s of the 20th century the finnish analytical chemist Yrjö Kauko investigated several
chemical methods to determine CO2 in gas mixtures and solutions. The Pettenkofer method and
several variants (pH-metric, colorimetric) were evaluated and solutions established that were used
until the 50s. worldwide. He developed a chemical method using cryogenic condensation achieving an
accuracy of 0,33% [Kauko 1935].
Yrjö Kauko 1886 –1974,
Analytical Chemist , Helsinki, Finland
Pioneer in developing analytical methods for determination of CO2 in
air and solutions
(Past 2008)
A simple volumetric gas analyser called „Kohlensäurebestimmungs-Apparat“ based on adsorption
showing extreme accuracy was designed by Paul Schuftan, one of the fathers of modern gas
adsorption chromatography [Hinshaw 2003] 1932 at the company of Linde together with Riedel & Co
in Essen (Germany). It was marketed as the Rico C [Schuftan 1933, Arnold et al. 1985, Kreutz 1941].
6
7
Paul Schuftan, (1896-1980) [B11]
German chemist, pioneer of gas chromatography, Linde (Germany)
and BOC (UK.
In honouring him: The BOC Memorial Schuftan Prize in chemical
engineering (UK) [Schuftan 1931, 1933, Arnold 1985, Hinshaw 2003]
Wilhelm Kreutz, director of the agricultural meteorological weather station at the periphery of Giessen
(Germany) used the Schuftan equipment to do the most accurate measurements of CO2 in air before
C.D. Keeling 1958.
During 1½ years from 1939 to 1941 Kreutz sampled
CO2 values of air every 1.5 hours at 4 distinct
heights above the ground (0m, 50 cm, 2m, 14m)
together with all important meteorological
parameters (radiation, precipitation, cloudiness,
wind, wind direction, pressure, temperature,
humidity). Each day about 120 samples were taken
and a total of about 64,000 samples were obtained
and measured.
Schuftan’s volumetric/manometric gas analyser
had an accuracy of 3 Vol % for all gases (e.g. O2,
H2O, CO2) and for CO2 the error was +- 1,5%
[Schuftan 1933 p. 514] . The gas analyser enabled
a time of analysis of 5 minutes with immediate
reading by capillary manometer.
The results were considered as a standard at that
time [Vaupel 2006].
Figure 2-4. “Kohlensäurebestimmungsapparat“
Riedel’s Rico C designed by
Schuftan 1932 [Schuftan 1933,
Riedel 1934]
In 1946 P.F. Scholander designed a compact volumetric gas analyser with an accuracy of 0.015
Vol% which was able to measure CO2 concentrations out of minimal air samples of 0.5 ccm in 6 –10
minutes. Compared to other methods cited Scholanders equipment accuracy was about 5-10 times
lower. Thousands of measurements were conducted using this equipment at sites round the globe; in
the Arctic, the Antarctic, the Tropics and on the top of Mount Everest.
P.F. Scholander (1905-1980 ), [B12]
Swedish physician and physiologist
Pioneer of blood gas measurement [Scholander 1943, 1947,NASA
1989]
Scholander’s equipment was later as the standard in medicine for levelling blood gases and was also
used in measuring respiration metabolism in plants and animals. By invitation of Roger Revelle who
7
8
was the director of the Scripps Institution of Oceanography in La Jolla, California, in 1952 P.F.
Scholander started work as a professor in physiology at the Scripps Institution. Today ecologists still
work with some equipment Scholander designed. NASA used the Scholander Gasanalyser up to
1998 in space craft.
For the sake of completeness, the physical method C. D. Keeling used from 1955 until 1958 should be
mentioned. In 1958 he began his measurements at Mauna-Loa that are described in section 2.1.
[Machta 1972, Keeling 1958, 1961], but from 1955 until he began his Mauna Loa studies he used a
method based on the URAS gas analyser invented 1938 at the BASF Company Germany.
K.F. Luft (1909-1999 ), Erwin Lehrer [B13]
German physicists
Inventors of the URAS, the first NDIR gas analyzer 1938
This analyzer was the first on-line continuous process gas analyzer. The URAS was based on a
photometer developed by K. Luft in 1937 to survey the Butadien synthesis at BASF (IG Farben). The
first apparature was designed to check CO in pure Hydrogenium for the synthesis of Ammonia
[Analytic Journal GmbH 2009].
The function of URAS is described by the following citation of Worthington 2009:
“This NDIR spectrometer operates according to the principle of negative filtering. Lehrer and Luft were
the first to use a microphonic pneumatic detector that also incorporated the sensitizing gas within the
detector.(10) Two nickel-chromium coils heated electrically to ca. 1000 K are used as radiation
sources. The radiation is modulated by a chopper which is formed like an aperture. A pneumatic
detector is used to detect the radiation and its two chambers are connected by a diaphragm capacitor.
The chambers are filled with the gas to be measured, usually diluted with N2. The sample cell is
flushed with this gas whilst the reference cell is filled with N2. If there is absorption of radiation in the
sample cell, the gas pressure in the sample chamber of the detector varies and the capacitance of the
diaphragm capacitor also changes at the modulation frequency. The resulting AC voltage is amplified,
rectified, and recorded.
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9
Fog. 2.5 URAS NDIR Gas Analyzer patented by Luft and Lehrer (BASF) 1938. On the left the two cell
arrangement with a sample cell and a reference cell. [Analytic Journal GmbH 2009].
The German company Hartmann & Braun got the rights to fabricate the URAS in 1952. The production
was ceased in 1986 after producing more than 1100 gas analyzers.
The accuracy of the first URAS equipment was limtited by the resolution of reading and was better
than 1%. CO2 concentrations of 0,00022 Vol % (2,2 ppm) could be detected. [Egle et al. 1951]
Charles Keeling had used later in 1958 a Siemens type of the URAS called Ultramat 3 to measure
CO2 at Mauna Loa and the south Pole station.
Since 1949 the URAS was used by German plant physiologists with great success to investigate
assimilation and respiration. [Egle et al. 1951]
In the early 50s the German biologists had used sulfuric acid or silica gel to free air from water.
Because there was a continous gas stream the sulfuric acid acts like a memory with a short
retardation for CO2 because of its absorption capacity. Thereby the absorbed CO2 is set free after a
short time and could be analysed in contrast to the sulfuric acid-drying of a fixed volume of air in the
gas analysers of some French scientists (Müntz and Reiset in the late 19th century).
To overcome these problems C. Keeling had used cryogenic condensation to condensate CO2
developed by Paul Schuftan in 1930 described in [Schuftan 1931], Craig 1953 and Glückauf 1944.
They had used cryogenic condensation of CO2 with liquid N2.
During 1944 in the grounds of Kew Gardens, England, Glückauf had determined the atmospheric CO2
concentration to be 333 ppm at ground level and 253 ppm at a height of 4-11 km above the ground by
using a balloon. Measurements he conducted on Imperial Tower College gave a value of 360 ppm.
Keeling modified Glückauf’s procedure and constructed a manometer for accurate determination of the
amount of CO2. By this method he sampled CO2 on the pacific coastline of USA from 1955 using a
sample time of several hours for each sample. He provides an accuracy of ± 1ppm = 0.3 % but
lateron carrier gas errors were known rising systematic error to 4 ppm. He collected other samples
over grassland, snow covered mountains, deserts and in forests show a CO2 and obtained results that
varied from 299 to >500 ppm. His averages were not arithmetical calculated but close to the lowest
values measured in the afternoon. This he named “background level”
9
10
Keeling conceded (Keeling 1958) that his early CO2 sampling from 1954/55 had been done
without literature studies. He did not mention P.F. Scholander’s gas analyser (results within
minutes) although Scholander had 10 years of experience in gas analysis worldwide and was
part of the staff of the Scripps Institute at that time. And he also did not mention Paul Schuftan
who was the leading expert in the world on gas analysis at that times.
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