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Experiment 2: Elemental Analysis by Sodium Fusion

Jirov A. Advincula, Adriel Noel R. Andonaque, Czariss Dale Grace A. Bedoya


Group 1, Chemistry 33 – LB5A Date Performed: September 20, 2019
Sir Aaron Noel P. Genato Date Submitted: October 11, 2019

Abstract
The determination of the presence of nitrogen, sulfur, and halogens in different organic
compounds cannot be done while these compounds are in their organic forms, but is possible if
these were converted into their inorganic anions which will bind with a cation. In this particular
qualitative analysis designed by Jean Louis Lassaigne, sodium was used to isolate these
elements from their covalence with carbon chains. Sodium fusion of p-chloroaniline, sulfanilic
acid, chlorobenzene and unknown compounds were separately conducted, and each extract was
tested for the presence of sulfur, nitrogen, and halogens. Positive and negative results for each
sample were deduced after observation of changes in color of the solution and appearance of
precipitate. The presence of nitrogen and the halogen chlorine was confirmed for p-chloroaniline.
Sulfanilic acid tested positive for both sulfur and nitrogen, while chlorobenzene tested positive
for chlorine. Thus, elemental analysis on p-chloroaniline, chlorobenzene, and sulfanilic acid
confirmed the presence of sulfur, nitrogen, and halogens, and the compositions of the set of
unknowns were partially revealed.

Keywords: qualitative analysis, sodium fusion, Lassaigne’s extract, sulfur, nitrogen, halogens

I. Introduction (Henssonow et al., 2010). Lassaigne started this


discovery with the detection of nitrogen from
The significance of elemental analysis in the field
samples of small quantities. He has observed
of organic chemistry has played a vital role in
that chemists before used to determine the
determining the composition of certain
presence of nitrogen in several reactions through
compounds, whether it be confirmatory or
isolating the proper substances in the gaseous
completely exploratory to of some of unknown
state. By burning the gas, nitrogen is transformed
(Gabbai et al., 2016). It can be done in two ways:
into ammonia, which is easily identified but not in
qualitatively and quantitatively. Qualitative
minimal amounts of the substance.
approach ascertains the presence of particular
elements, but the percent amount (usually in In Lassaigne's fusion experiment of nitrogen-
percent weight) is done quantitatively (Barron & containing organic compound and potassium
Raja, 2019). For instance, according to Borje and produced potassium cyanide, he discovered that
Hall (2001), in determining the amount of carbon in the presence of ferrous-ferric salt, the
and hydrogen in an organic compound, these are precipitate was green blue or yellow and after a
converted to carbon dioxide and water through few drops of HCl, the precipitate turned blue. He
combustion followed by a quantitative analysis of continued his experiment with other nitrogen-
the latter compound. In the field of a more containing organic compounds in small
advanced technological analysis, most common quantities. Using the same method of fusion and
techniques used in laboratories today are X-ray the addition of ferrous-ferric sulfate followed by a
fluorescence (XRF), absorption atomic drop of HCl, the presence of nitrogen was
spectroscopy (AAS), and inductively coupled indicated by the formation of a deep blue solution
plasma (ICP) techniques (Bozic, 2019). (Wisniak, 2014). However, it was Jacobsen in
1897 who replaced potassium with sodium as the
However, the experiment was only limited to
active reagent since sodium is a stronger
qualitative analysis, which was specifically done
reducing agent than potassium (Gower &
through Lassaigne’s test, considered to be the
Rhodes, 1969). This fusion method was then
most efficient method in laboratories (Criddle and
developed by other scientists to detect other
Ellis, 1967). Also known as the sodium fusion
elements such as halogens and sulfur (Wisniak,
test, this particular experimental setup is named
2014). Other elements, aside from nitrogen,
after its developer, Jean Louis Lassaigne
sulfur and halogens, are usually only tested if

Chemistry 33: Elemental Analysis by Sodium Fusion Page 1 of 11


their presence is suspected from other evidence funnel. This procedure was separately done for
(Gower & Rhodes, 1969). the preparation of sodium fusion with p-
chloroaniline, sulfanilic acid, chlorobenzene, and
The sodium-fusion test usually makes use of
an unknown substance respectively.
color changes or precipitate formation in
solutions to indicate specific chemical reactions Sulfur Test
(Co & Salindo, 2012). The test involves “fusing”
Five drops of the prepared fusion solution was
clean sodium metal with an organic compound
added into a 10-mL test tube containing three
sample at very high temperature (Henssonow et
drops of water. Two drops of 2% aqueous
al., 2010). The main principle is that, since
Na2[Fe(C)5NO] was then added to the solution.
elements to be tested are covalently bonded to
Development of a purple solution indicated a
the hydrocarbons, their tendency is to break the
positive result; absence of sulfur in the sample
bond with the carbon chains, becoming in their
was deduced otherwise.
ionic form (which are anions in this case) to bond
with the cation metal Na+. These new ionic bonds Nitrogen Test
are extracted from the “fused” mass by boiling
and subsequent filtering. The extract, called a A pinch of FeSO4 was added to a test tube
sodium fusion extract or Lassaigne’s extract, is containing 1 mL of the fusion solution. Five drops
subjected to different qualitative tests utilizing of 10% KF was also added, and the solution was
different reagents to specifically identify if the boiled for 10 seconds. After boiling, two drops of
sample contains nitrogen, sulfur, and/or 5% FeCl3 was added to the solution, and 6 M
halogens (vlab.amrita.edu, 2011). H2SO4 was added to acidify the solution. A piece
of litmus paper was dropped into the solution to
The objectives of the experiment were to (1) confirm the acidity of the solution. Development
prepare a “complete” sodium fusion of p- of a blue solution confirmed the presence of
chloroaniline, sulfanilic acid, chlorobenzene, and nitrogen; similar to the previous test, absence of
unknown samples; (2) distinguish a positive nitrogen is indicated otherwise.
result from a negative result in respective
analyses using compounds of known elemental Halogen Test
composition; and (3) determine whether the sets In a fume hood, a test tube containing 10 drops
of unknown compounds contain nitrogen, sulfur, of the prepared fusion solution and a few drops
chlorine, bromine, and/or iodine. of 2M HNO3 was heated. After subjecting to heat
II. Experimental for five minutes, four drops of 0.1M AgNO 3 was
added. The test tube was then centrifuged at
Sodium Fusion 1000 rpm for one minute. The decantate was
discarded from the test tube, and 2 M NH3 was
In a fume hood, a 5 mm piece of sodium metal
added dropwise to the test tube to examine its
was removed from a kerosene oil bath and then
solubility. The properties of the formed precipitate
placed on tissue paper and patted dry. A few
(if any) were observed to deduce the presence of
drops of hexane were used to remove excess
halogens.
kerosene and to ensure sodium purity. The
sodium was then placed in a test tube and heated III. Results
over an alcohol lamp until the metal had
vaporized. The test tube was removed from the Since the experiment used a qualitative
flame and 30 mg of the organic sample was approach in elemental analysis, the sets of
added into the tube. The test tube was then again results are descriptive observations on the color
heated for ten minutes. While still hot, the test change, precipitation and the corresponding
tube was dropped into a 150-mL beaker appreciable solubility of the precipitates formed.
containing approximately 20 mL of distilled water Supplemental figures are attached in the
allowing it to break and have the fusion mix with Appendices.
the water. The solution in the beaker was again
heated for five minutes, after which it was filtered
into another beaker using filter paper in a glass

Chemistry 33: Elemental Analysis by Sodium Fusion Page 2 of 11


Sodium Fusion Nitrogen Test

Table 1. Color appearance of sodium fusion Table 3. Color appearance of the solution after
extract after filtration. nitrogen test.
Sample Color of Solution Color of
Sample Indication
p-chloroaniline slightly grayish Solution
chlorobenzene slightly grayish p-chloroaniline light blue +
sulfanilic acid colorless chlorobenzene cloudy yellow -
unknown 1 yellowish sulfanilic acid blue* +
unknown 2 slightly grayish unknown 1 dirty yellow -
unknown 3 slightly grayish unknown 2 dark brown -
unknown 5 yellowish unknown 3 dark orange -
unknown 6 colorless unknown 5 faint yellow -
unknown 7 colorless unknown 6 dark green -
unknown 7 dark green -
As shown in Table 1, both the p-chloroaniline and *after a period of time, dark blue precipitate was
chlorebenzene solutions were slightly grayish, formed and the solution turned colorless
while the fusion solution of sulfanilic acid was
Nitrogen is present in p-chloroaniline and
colorless.
sulfanilic acid due to blue coloration of their
Most of the unknown samples had a grayish solution after the addition of FeCl3. However, the
appearance similar to the previous fusion solution in containing sulfanilic acid turned into
solutions except for unknowns 1, 5, 6, and 7. colorless as dark blue precipitate formed and
Unknown samples 1 and 5 were both yellowish, settled at the bottom of the tube. P-chloroaniline
while the solutions for both Unknowns 6 and 7 contrastingly didn’t exhibit this aftermath and
were colorless. There was no unknown 4 since remained blue the entire time. On the other hand,
the experiment on this sample wasn’t completely chlorobenzene and unknown 1 exhibited
conducted. yellowish coloration of the solution, a negative
response to nitrogen testing. Unknown 1 was
Sulfur Test described as “dirty” due to the presence of black
precipitate-like particles. None of the unknowns
Table 2. Color appearance of the solution after responded positively to nitrogen testing, since
sulfur test. none has turned blue.
Color of
Sample Indication
Solution Halogen Test
p-chloroaniline deep yellow -
chlorobenzene deep yellow - Table 4. Color of the precipitate formed after the
deep blue- addition of AgNO3 and their solubility in NH3.
sulfanilic acid +
violet
Color of Solubility
unknown 1 deep yellow - Sample
Precipitate in NH3
unknown 2 brown -
slightly
unknown 3 yellow - p-chloroaniline white
soluble
unknown 5 purple +
chlorobenzene none N/A
unknown 6 dark yellow -
sulfanilic acid black* N/A
unknown 7 yellow -
unknown 1 none N/A
unknown 2 none N/A
As table 2 suggests, p-chloroaniline, unknown 3 none N/A
chlorobenzene, and unknown 1 responded unknown 5 none N/A
negatively in the sulfur test, indicated by deep slightly
unknown 6 yellow
yellow coloration. However, sulfanilic acid fusion soluble
solution turned blue violet, which is a positive unknown 7 none N/A
indication of sulfur. Among the remaining *black precipitate is a nonhypothetical result,
thus there is no need to check its solubility
unknowns, unknown 5 exhibited a similar result
with sulfanilic acid, suggesting a positive result as
Upon addition of AgNO3, only the p-chloroaniline
well.
precipitated and is slightly soluble in NH3.
Chlorobenzene, however, appeared to have a

Chemistry 33: Elemental Analysis by Sodium Fusion Page 3 of 11


cloudy yellow solution, which can be an indication Additionally, heating volatilizes any unreacted
of incomplete precipitation. On the other hand, organic material from the sample compound in
sulfanilic acid accumulated black precipitate, order to avoid disturbances in the results. When
which is different from the expected outcomes the ignition tube was red-hot, it was plunged into
(which could either be white or yellow a beaker containing distilled water and covered
precipitate), so the solubility of this precipitate with wire gauze in order to secure the products in
was not tested anymore. Among the unknown, the aqueous solution. Reheating is an optional
unknown 6 exhibited yellow precipitation and is process but hotter solutions are easier to filter
slightly soluble as well. than colder ones. The filtrate at this point, which
is supposed to be colorless (otherwise indicating
IV. Discussion an incomplete fusion reaction), is the sodium
fusion extract, or Lassaigne’s extract, which
The paradigm of Jean Louis Lassaigne on
contains the inorganic compounds if present and
sodium fusion has a goal of breaking the organic
will be subjected to different qualitative testing to
covalent bonds between hydrocarbons and
detect the presence of sulfur, nitrogen, and
functional groups which contain the elements to
halogens (Gower & Rhodes, 1969).
be tested to form new inorganic compounds
which display color changes during reactions. In organic compounds containing both nitrogen
Sulfur-containing groups are usually bonded with and sulfur, sodium metal as mentioned must be
carbon chains as sulfonic acids, thioaldehydes, excessive in order to prevent the mechanism
thioketones, thiols, and sulfides. Nitrogen is shown in Eq’n 4, where sodium thiocyanate is
mostly contained in amide, nitrile, amine, and formed after combining nitrogen and sulfur in a
nitro compounds. Lastly, halogens such as single compound (sodium thiocyanate). But,
chlorine, bromine, and iodine are bonded to excessive sodium will favor the reactions in Eqn’s
carbons as halides or acyl halides. These organic 1 and 2 rather than the reaction in Eq’n 4
molecules bind these specific elements or groups (vlab.amrita.edu, 2011). With that, sulfur and
covalently. However, these bonds are easily nitrogen tests can be done separately.
broken by sodium, which is a very strong
reducing agent and can break the organic [Eq’n 4] Na+ + CN- + S2- → NaSCN(aq)
compound chain (Kokv, 2011). When these Sulfur Test
elements separate from their respective organic
compounds, the tendency is to exist in their [Eq’n 5] Na2S(aq) + Na2[Fe(CN)5NO](aq) →
stable ionic form, such as S2-, CN-, Cl-, Br-, and I- Na4[Fe(CN)5NOS](aq)
, by which the elements may ionically bind with
As illustrated in Eq’n 1, sulfur exists in the
Na+ during fusion. There must be an excess of
solution as sodium sulfide. During sulfur testing,
sodium metal in order for the reaction to proceed
the addition of 2% sodium nitroprusside results to
towards the formation of ionic compounds. The
a combination reaction forming sodium
newly formed inorganic compounds are then
pentacyanonitrosylferrate (II) (as shown in Eq’n
suspended in the aqueous solution and are
5). Sodium pentacyanonitrosylferrate (II) appears
subjected to different reactions during qualitative
in the solution as deep blue-violet in color
testing. Combination reactions such as in ionic
(Shriner et al., 2004).
bonding are illustrated below (Shriner, Hermann,
Morrill, Curtin, & Fuson, 2004). Of the three known compounds, only sulfanilic
acid responded positively to the test, while p-
[Eq’n 1] 2 Na+ + S2- → Na2S(aq)
chloroaniline and chlorobenzene exhibited a
[Eq’n 2] Na+ + CN- → NaCN(aq) deep yellow coloration. Theoretically, these
results are correct since sulfanilic acid contains
[Eq’n 3] Na+ + X- *→ NaX(aq)* sulfonic acid functional groups (-SO3H) as shown
*where X is any halide i.e. in Figure 1 below, whilst the other two
chloride, bromide, or iodide compounds lack sulfur. Similarly, unknown 5 has
During sodium fusion reaction, heating is an also a positive result, which suggests that it must
important process and is vital in order to push the have sulfur.
reaction forward as shown in Eq’ns 1, 2, and 3.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 4 of 11


In the experiment, p-chloroaniline and sulfanilic
acid tested positive since the organic structures
of both compounds contain amine groups,
illustrated in Figures 2 and 1, respectively.
Meanwhile, chlorobenzene exhibited a cloudy
Figure 1. Structure of 4-aminobenzenesulfonic acid yellow color. Unknown 1 exhibited a dark yellow
(sulfanilic acid). Adapted from “Why do we change coloration as well, which suggest a negative
sulphanilic acid to a zwitterion? Why does sulphanilic
response for these two in nitrogen testing.
acid exist as a zwitterion?” by quora.com (2019).
Meanwhile, unknown 7 encountered a greenish
Nitrogen Test precipitate. This indicates that the sodium wasn’t
heated enough during fusion, that is why there
[Eq’n 6] 2 NaCN(aq) + FeSO4 (s) → was only a very minute amount of cyanide that
Fe(CN)2 (aq) + Na2SO4 was detected (Kokv, 2011). This result is
[Eq’n 7] Fe(CN)2 (aq) + 4 NaCN(aq) → commonly encountered in early practices, so, as
Na4Fe(CN)6 (aq) discussed, the convention of adding KF to the
solution yields a more desirable data upon
[Eq’n 8] Na4Fe(CN)6 (aq) + 4 KF(aq) → completion.
K4Fe(CN)6 (aq) + 4 NaF

[Eq’n 9] 3 Na4Fe(CN)6 (aq) + 4 FeCl3 (aq) →


Fe4[Fe(CN)6]3 (aq) + 12 NaCl

[Eq’n 10] K4Fe(CN)6 (aq) + FeCl3 (aq) →


KFe[Fe(CN)6](s) + 3 KCl Figure 2. Structure of 4-chloroaniline (p-
chloroaniline). Adapted from “4-chloroaniline” by
Eq’n 2 illustrates that nitrogen group in a sodium
Toronto Research Chemicals (n.d.).
fusion exist as sodium cyanide. Upon addition of
ferrous sulfide, sodium will be displaced from the Halogen Test
compound to form ferrous cyanide (Eq’n 6).
Ferrous cyanide will further react and combine [Eq’n 11] NaCN + Na2S + 3 HNO3 → heat

with the remaining sodium cyanide in the solution HCN(g) + H2S(g) + 3 NaNO3 (aq)
to form sodium ferrocyanide (Eq’n 7). Addition of [Eq’n 12] NaX + AgNO3 (aq) →
Ksp

potassium fluoride in the solution complexes with AgX(s) + NaNO3 (aq)


sodium ferrocyanide, forming potassium
ferrocyanide (Eq’n 8). Upon the addition of ferric [Eq’n 13] AgCl(s) + 2 NH3 (aq) ↔
chloride, both the remaining sodium ferrocyanide [Ag(NH3)2]+(aq) +Cl-(aq)
(Eq’n 9) and potassium ferrocyanide (Eq’n 10) In a halogen test, the goal is to precipitate any
will react and form ferric ferrocyanide and present halogen with silver (as shown in Eq’n 12).
potassium diiron (III) hexacyanoferrate, However, other organic compounds may contain
respectively (Haynes, 1966; Brainly, 2018). Early other elements or groups that can complex with
practice in nitrogen testing did not include the silver and form a precipitate (in this case,
addition of KF, which is why earlier studies did nitrogen and sulfur). The addition of nitric acid to
not always acquire the most accurate qualitative the solution favors the reaction involving sulfides
results in this particular test. However, the and cyanides of forming hydrogen sulfide and
presence of potassium diiron (III) hydrogen cyanide, respectively and as shown in
hexacyannoferrate is confirmed by dark blue Eq’n 11. The two aforementioned acids are weak
precipitate, specifically Prussian blue (Brainly, acids that volatilize upon heating. It is possible
2018). Thus, collectively, the products formed that this mechanism may involve formation of
after addition of ferric chloride provide a HCl, HBr, and HI. However, these are strong
qualitative amount upon determination of acids in comparison with the weak acids which
nitrogen presence, which is deduced if Prussian will evaporate first when heated. Upon the
blue precipitate settles at the bottom of the tube addition of silver nitrate, the halogens present will
after the blue coloration of the solution vanishes. favor precipitation. Ksp values of these halogens

Chemistry 33: Elemental Analysis by Sodium Fusion Page 5 of 11


are really small, so their precipitate complex is solution completely. Those black precipitates are
more favorable in the reaction. This approach in silver sulfides. On the other hand, the yellow
halogen testing is particular to chloride, bromide, precipitation on unknown 6 is a false positive
and iodide only due to their capacity to be attract result since it is expected not to exhibit any
a relatively large molecule (i.e. Ag+) and not precipitation. One possible source of
dissociate easily. This is why AgF can no longer precipitation is the incomplete expulsion of non-
be included in the scope because it is highly halogen elements (which was previously
soluble and can only accumulate very minute to discussed). Unknown 3 must have contained
no amount of precipitate (quora.com, 2014). In positive result indicating presence of chlorine, but
order to detect if there are any halogens present possible mishandling of the procedures might
aside from the three, other tests must be have further expelled them as well.
conducted using other reagents.

To distinguish which halogen is present, the color


and solubility in NH3 of precipitate are observed
and tested (Table 5).

Table 5. Color of halide precipitate and their Figure 3. Structure of 1-chlorobenzene. Adapted
solubility in NH3. from “Difference Between Chlorobenzene and Benzyl
Color of Solubility in Chloride” by Madhusha (2018).
Halogen
Precipitate NH3
chlorine white soluble V. Conclusion and Recommendations
bromine yellow slightly soluble
Elemental analysis confirmed the presence of
iodine yellow insoluble
expected elements in the known compounds.
Silver chloride is a white precipitate and is soluble Sulfanilic acid tested positive for both sulfur and
in NH3. As shown in Eq’n 13, the complexation nitrogen. p-chloroaniline produced a positive
reaction of silver chloride with ammonia is result for both nitrogen and halogen tests, and
reversible, but the formation of the complex is the halogen was then identified as chlorine.
more stable, thus the reaction is more favorable Lastly, chlorobenzene tested positive for
towards forward reaction. On the other hand, halogens, of which chlorine was identified.
silver bromide appears to be yellow and slightly Of seven unknown samples subjected to the
soluble in NH3 as well but is soluble in more three elemental analysis tests, only unknown 5
concentrated NH3. Lastly, silver iodide is also tested positive for sulfur, while only unknown 6
yellow in color, but is insoluble due to its very low tested positive for halogens. The halogen was
solubility constant (Clark, 2015; Shriner et al., identified to be bromine. However, some
2004). Centrifugation prior to solubility testing discrepancies were identified between the
separates the precipitate from the solution and expected results and the obtained data. First,
allows for easy decantation. unknown 3 was expected to test positive for
During halogen testing in the experiment, p- halogens, specifically chlorine. This is an
chloroaniline and chlorobenzene (chloride- indication that the halogen did not completely
containing as shown in Figure 3 below) both react with sodium during fusion. The same case
produced a white, soluble precipitate, while, was found for unknown 7, where nitrogen was
sulfanilic acid produced black precipitate. This is expected to be present. The halogen test result
an undesired result because upon precipitate for unknown 6 was a false positive, as it did not
formation, the presence of nitrogen and sulfur in contain any of the testable elements within the
the solution might affect the results afterwards. scope of the study.
Silver cyanide can be mistakenly observed as It should be noted that the study was only limited
silver chloride, because it also appears as white to the elemental analysis of nitrogen, sulfur, and
precipitate. However, silver sulfide appears to be halogens, and therefore did not provide
black. This is observed in sulfanilic acid, which comprehensive information regarding the full
suggests that the nitric acid added and the composition of the given analytes. It is
process of heating did not expel the sulfide in the recommended to conduct further studies utilizing

Chemistry 33: Elemental Analysis by Sodium Fusion Page 6 of 11


tests that will allow the determination of the Haynes, B. (1966). Qualitative Organic Analysis.
presence of other elements not included in the 762-766.
study. Qualitative analysis also did not obtain Henssonow, S. F., Surhone, L. M., Tennoe, M. T.
data pertaining to the amount of any specific (2010). Sodium Fusion Test. Retrieved 3
element contained in the given analytes. This October 2019 from https://www.betterworld
may be resolved by using quantitative methods books.com/product/detail/sodium-fusion-
in future studies to determine the amount of each test-6132972609
element present in the respective analytes in Madhusha. (2018). Difference Between
discrete quantities. Chlorobenzene and Benzyl Chloride.
Retrieved 10 October 2019 from https://
VI. References pediaa.com/difference-between-chlorobenz
Barron, A. R. & Raja, P. M. V. (2019). ene-and-benzyl-chloride/
Introduction to Elemental Analysis. Retrieved Kokv, G. (2011). Qualitative Analysis of Organic
3 October 2019 from https://chem.libretexts. Compounds (Sodium Fusion Test or
org/Bookshelves/Analytical_Chemistry/Book Lassaigne’s Test). Retrieved 10 October
%3A_Physical_Methods_in_Chemistry_and 2019 from http://1chemistry.blogspot.com
_Nano_Science_(Barron)/01%3A_Elementa /2011/12/qualitative-analysis-of-organic.html
l_Analysis/01.1%3A_Introduction_to_Eleme
ntal_Analysis. quora.com. (2014). Why is the solubility product
of AgCl>AgBr>AgI? Retrieved 10 October
Börje, S. & Hall, A. J. (2001). Techniques and 2019 from https://www.quora.com/Why-is-
Instrumentation in Analytical Chemistry. the-solubility-product-of-AgCl-AgBr-AgI
Molecularly Imprinted Polymers: Man-made
Mimics of Antibodies and their Applications in quora.com. (2019). Why do we change
Analytical Chemistry. Volume 23, 21-57. sulphanilic acid to a zwitterion? Why does
sulphanilic acid exist as a zwitterion?
Bozic, Dunja. (2019). Most Common Elemental Retrieved 10 October 2019 from
Analysis Techniques. AZoM. Retrieved 3 https://www.quora.com/ Why-do-we-change-
October 2019 from https://www.azom.com/ sulphanilic-acid-to-a-zwitterion-Why-does-
article.aspx?ArticleID=16423. sulphanilic-acid-exist-as-a-zwitterion
Brainly (2018). What happens when ferric Shriner, R., Hermann, C., Morrill, T., Curtin, D.,
chloride is added to potassium ferrocyanide. Fuson, R. (2004). The Systematic
Retrieved 7 October 2019 from https:// Identification of Organic Compounds.
brainly.in/question/ 7314292 Hoboken, NJ: John Wiley & Sons, Inc. 53-60.
Clark, J. (2015). Testing for halide ions. Toronto Research Chemicals. (n.d.). 4-
Retrieved 10 October 2019 from https://www. chloroaniline. Retrieved 10 October 2019
quora.com/Why-is-the-solubility-product-of- from https://www.trc-canada.com/product-de
AgCl-AgBr-AgI tail/?CatNum=C377500
Co, F. A. K. & Salindo, E. S (2012). Experiment vlab.amrita.edu. (2011). Detection of Elements:
#6: Elemental Analysis. Retrieved 3 October Lassaigne’s Test. Retrieved 3 October 2019
2019 from https://www.scribd.com/doc/867 from vlab.amrita.edu/?sub=2&brch=191&s
37439/Exp-6-Sodium-Fusion-PDF im=344&cnt=1.
Criddle W.J. & Ellis G.P. (1967). Preliminary Wisniak, J. (2014). Jean Louis Lassaigne.
Tests. In: Qualitative Organic Chemical Retrieved 7 October 2019 from https://
Analysis. Springer, Boston, MA. revista.cnic.edu.cu/revistaCB/articulos/jean-
Gabbai, F. P., Chirik, P. J., Fogg, D. E., Meyer, louis-lassaigne.
K., Mindiola, D. J., Schafer, L. L., You, S.
(2016). An Editorial About Elemental
Analysis.Organometallics. 35, 3255-3256. Appendices: Actual Figures
Gower, R. & Rhodes I. (1969). A Review of The following appendages in this paper are
Techniques in the Lassaigne Sodium- images taken during the conduct of experiment.
Fusion. Journal of Chemical Education, Vol. It is divided into four parts: photos for (1) sodium
46 No. 9. 606-607. fusion extraction, (2) sulfur testing, (3) nitrogen
testing, and (4) halogen testing.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 7 of 11


Appendix A: Sodium Fusion

Figure 6. Dropping of test tube into a 150-mL


beaker containing approximately 20 mL of
Figure 4. Sodium metal in a test tube.
distilled water allowing it to break and have the
fusion mix with the water.

Figure 7. Boiling of the solution for five minutes.


Figure 5. Heating of the sodium metal before
adding a sample.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 8 of 11


Figure 8. Sodium fusion extract (p-chloroaniline Figure 10. Sulfanilic acid responding positively
as sample), also known as Lassaigne’s extract, in the sulfur test, indicated by deep blue-violet
after filtering. coloration.

Appendix B: Sulfur Test

Figure 11. Unknown 1 responding negatively to


Figure 9. P-chloroaniline responding negatively the sulfur test, indicated by the deep yellow
in the sulfur test, indicated by deep yellow coloration.
coloration.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 9 of 11


Appendix C: Nitrogen Test solution, turned colorless and deposited blue
precipitates after a few minutes (14).

Figure 12. P-chloroaniline responding positively


in the nitrogen test, indicated by the light blue Figure 15. Unknown 1 responding negatively to
coloration. the nitrogen test, indicated by the dirty yellow
coloration.

Appendix D: Halogen Test

Figure 13 (up) & 14 (down). Sulfanilic acid Figure 16. P-chloroaniline responding positively
responding positively to the nitrogen test, to the halogen test, indicated by the white
indicated by the blue coloration (13). But the precipitate that is slightly soluble with NH3.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 10 of 11


Note: The photos were not complete for all
samples because (1) groups who worked on
chlorobenzene were not able to take photos and
(2) series of earthquakes was happening during
the experiment which caused a large distraction
to the students.

Figure 17. Sulfanilic acid responding negatively


to the halogen test, indicated by the absence of
white or yellow precipitate but an accumulation
of black precipitate (silver sulfide).

Figure 18. Unknown 1 responding negatively to


the halogen test, indicated by the absence of
precipitate.

Chemistry 33: Elemental Analysis by Sodium Fusion Page 11 of 11

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