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The ‘Maybrick Diary’ Ink

The ‘Maybrick Diary’ Thin Layer Chromatography Analysis

Thin Layer Chromatography

Thin Layer Chromatography (TLC) is a way to identify compounds in a mixture[1]. ‘A small spot of solution containing the sample is applied to a plate, about one centimetre from the base. The plate is then dipped into a suitable solvent, such as ethanol or water, and placed in a sealed container. The solvent moves up the plate by capillary action and meets the sample mixture, which is dissolved and is carried up the plate by the solvent’[2]. The different compounds in the sample have differences in rates of solubility in the solvent and differences in ‘their attraction to the stationary phase’, this means they travel at different rates[3]. ‘The separations will probably be colourless and must be visualised under ultraviolet light. Alternatively the slide can be sprayed with a suitable reagent which will cause the “trail” to become coloured’[4].

Thin Layer Chromatography (TLC) Analysis of ‘Diary’ Ink – Results

There have been three TLC analyses of the ‘Diary’ ink. The first of these was conducted by Dr Baxendale in 1992[5]; some TLC work was carried out by Dr Eastaugh in 1993[6] and in 1993 the Rendell team used TLC to duplicate Eastaugh’s work[7].

Baxendale’s TLC work looked at both the ‘Diary’ ink and paper separately[8]. The paper was examined ‘to establish  whether this contained anything which might confuse the observed findings from the ink’ as well as this Baxendale also examined ‘samples of ink from known documents of 1908 and 1925 and a selection of modern black inks’[9]. His analysis found that the ‘Diary’ ink was readily soluble and that only a small amount of insoluble residue was left on the paper. He stated that ‘the chromatogram showed only a partial separation: much of the ink remained on the baseline but there was a strip of partially resolved coloured components and a few colourless fluorescent spots. This pattern is characteristic of inks based on a synthetic dye called nigrosine’[10].  The paper sample ‘contributed no recognisable components to the chromatogram’[11]. In relation to the comparison ink samples Baxendale noted that the 1908 and 1925 samples were both ‘virtually insoluble’ and so no chromatogram was obtainable and of the modern inks he noted that ‘one described as “calligraphic ink” was generally similar to the ink of the diary, and appeared to have individual components in common. Indian inks were less soluble and showed virtually no chromatographic separation.[12]

Eastaugh also carried out a TLC analysis alongside other microchemical techniques in order to ‘characterise certain components within the ink’[13]. Eastaugh stated ‘the principal microchemical technique employed here was to observe the colour changes that occurred when certain reagents were added to samples. This was a widely used approach for the study and interpretation of natural and synthetic dyes present in textiles, paints and inks’[14]. He found that when several samples of the  ‘Diary’ ink were tested using reagents such as ammonia and concentrated sulphuric acid ‘little reaction was observed, suggesting that the ink is not based on a synthetic dyestuff; however, low levels of a synthetic dye might not be revealed by this approach[15].’

Robert Kuraz, a member of the Rendell team in America, used TLC ‘to analyze the ink for any elements that would be inconsistent with the date [1888/9] and found none (he basically duplicated the work of Dr Eastaugh)[16]’.


The ‘Maybrick Diary’ SEM/EDX Analysis

SEM/EDX

SEM/EDX (Scanning Electron Microscopy/Energy Dispersive X-ray microanalysis) is a process whereby a finely focused beam of electrons is scanned onto a sample. These electrons interact with the molecular composition of the sample[17]. According to Forensicevidence.net ‘a series of measurable electron energies can be produced which are analyzed by a sophisticated microprocessor that creates a pseudo three dimensional image or spectrum of the unique elements that exist in the sample analyzed[18].

The SEM/EDX analysis can detect all elements from Carbon (atomic number = 6) upwards[19]; this means that it cannot detect elements with the atomic numbers 1-5, namely, Hydrogen (1), Helium (2), Lithium (3), Beryllium (4) and Boron (5). It can detect, in a quantitative analysis of bulk materials, elements in quantities greater than 2 micrometers and, in a qualitative analysis, those greater than 0.2 micrometers[20].

SEM/EDX is a difficult means to detect other elements with low atomic numbers including Carbon (6), Nitrogen (7) and Oxygen (8)[21].


SEM/EDX Analysis of ‘Diary’ Ink – Results

There have been two SEM/EDX tests carried out on the ‘Diary’ one by Dr Nicholas Eastaugh in 1992[22] and one by Leeds University in 1994[23]. These tests can tell us something about the elemental composition of the ink in the ‘Diary’.

The Eastaugh Report showed the following elements to be present in the ‘Diary’ ink:-

-         As a major constituent - Silicon, Sulphur and Aluminium

-         As a minor constituent - Sodium, Iron, Calcium and Potassium

-         As a trace – Magnesium, Chlorine, Phosphorus, Calcium and Potassium[24].

Eastaugh also found that the underlying shape of the spectra beneath the peaks implied the presence of ‘a significant low atomic weight component such as an organic base’[25]. No component was detected which would preclude a Victorian date[26], but this does not mean the ink is Victorian merely that it could be[27].

The Leeds Report showed the following elements to be present in the ‘Diary’ paper and ink:-

-         As principal ingredients - Sulphur, Silicon and Aluminium

-         As secondary constituents – Iron, Potassium, Calcium, Carbon, Oxygen and Chlorine

-         And also small amounts of Magnesium[28]

There were increased amounts of Iron and Sulphur in the ink and paper as to the paper only sample[29].

SEM/EDX Comparison of Victorian Inks

The Leeds team examined inks known to be from 1881 and 1887 using SEM/EDX. They examined a paper only and ink and paper sample from both documents[30]. In relation to the 1881 document the results showed that Iron and Sulphur were both present in the document’s ink in a significantly increased amount as compared to the paper only sample[31]. The results from the analysis of the 1887 document showed Iron to be present only in the ink and paper combination[32]. There was also a significant increase in the amount of Sulphur in the ink and paper sample as compared to the paper only sample as well as an increased amount of Potassium in the ink and paper sample[33].  The Leeds team noted that ‘the results obtained from the EDX analysis of the two documents are identical (in respect of the material) to those obtained for the ‘Ripper Diaries’ (see report number 1) i.e. the presence of an iron peak alongside a significant increase in the sulphur content’ they concluded ‘this suggests strongly that all three inks are of the Iron Gallotannate type’[34]


SEM/EDX Comparison of ‘Modern’ Inks

Eastaugh examined four modern black inks, these were, Mont Blanc, Quink, Watermans and Windsor and Newton drawing ink[35]. The results were that Mont Blanc did not match the ‘Diary’ as it contains no Iron (present in the ‘Diary’ ink) but did contain Iodine (not present in the ‘Diary’ ink). Quink had not contained Iron for ten years, Watermans contained ‘little Aluminium and Silicon’ and higher levels of Chlorine compared to the ‘Diary’ ink, whilst Windsor and Newton drawing ink did not contain as much Sulphur as the ‘Diary’ ink[36].There were therefore differences between all four of the modern inks and the ‘Diary’ ink.

Eastaugh advised caution in interpreting such results saying ‘I would not want to say on this basis that the diary ink is not modern – there is a basic similarity of composition under SEM/EDX between a number of the samples with no great outstanding feature which marks the Victorian from the modern[37]’.


The Elemental Composition of Diamine Black Manuscript Ink

It is alleged that the ‘Diary’ was forged using Diamine Black Manuscript Ink (Diamine Ink). Diamine Ink contains the following elements only:-

Carbon – this is a major constituent of all the organic compounds and is also present in a small amount as an elemental constituent of the Artilene Black pigment paste,

Oxygen – this is major constituent of everything in the ink,

Hydrogen – this is a major constituent of all the organic compounds in the ink,

Sulphur – this is a major constituent of the Ferrous Sulphate and a minor constituent of the Nigrosine (a dyestuff), 

Iron – this is a major constituent of the Ferrous Sulphate,

Nitrogen – this is a major constituent of the Nigrosine,

Chlorine – this is a constituent of Chloracetamide (a preservative) in the ink,

Sodium – this is a minor constituent of the Nigrosine.[38]

 

The Elements of Diamine Ink as to the Elements from the SEM/EDX ‘Diary’ Ink

The ‘Diary’ ink (as determined by the results of the two SEM/EDX tests) and Diamine Black Manuscript Ink (Diamine Ink) appear to have these elements in common, Sulphur, Iron, Sodium, Carbon, Chlorine and Oxygen[39].

Hydrogen (present in Diamine Ink[40]) would not be found by a SEM/EDX analysis since it has an atomic number lower than 6 (Hydrogen = atomic number 1)[41].

Due to their low atomic weight the SEM/EDX tests may have had trouble detecting both Oxygen (atomic number = 8) and Carbon (atomic number = 6)[42]. However, Oxygen and Carbon both showed up in the Leeds analysis[43] whilst Eastaugh stated that the underlying shape of the spectra beneath the peaks could imply the presence of significant low atomic weight components such as an organic base[44]; this would be consistent with Carbon and/or Oxygen being in the ink.

Nitrogen (present in Diamine Ink[45]) might be hard to detect using the SEM/EDX method because:-

(a)    it has a low atomic number (Nitrogen = atomic number 7)

(b)   The presence of Iron in the sample (Iron is present in the ‘Diary’ ink[46]) could have masked the presence of Nitrogen (if it is there) because of the similarities between the secondary electrons in Iron and the electrons in Nitrogen[47].

Sodium (present in Diamine Ink[48]) was detected in the ‘Diary’ ink by the Eastaugh SEM/EDX analysis[49] (whilst the Leeds SEM/EDX analysis detected no Sodium[50]). The Sodium content of Diamine Ink is derived solely from the Nigrosine, of which it is a minor constituent[51]. Therefore, there is only a very small amount of Sodium in Diamine Ink meaning the amount would probably fall below the lower detection limit for SEM/EDX analysis[52]. Therefore the presence of Sodium as a secondary constituent of the ‘Diary’ ink as found by Eastaugh’s analysis cannot be accounted for solely by any Nigrosine that may be present in the ‘Diary’ ink (and the fact that Leeds found no Sodium in their SEM/EDX analysis does not show that the ink contained no Nigrosine). For Sodium to have been detected by Eastaugh in the levels it was the ‘Diary’ ink has to contain a source of Sodium in addition to any Nigrosine, Diamine Ink contains no such source[53].

Chlorine at the levels in Diamine Ink would not show on a SEM/EDX analysis. This is as the Chlorine content of Diamine Ink is derived solely from its Chloracetamide and this level of Chlorine would probably fall below the detection limit of SEM/EDX[54]. It could be that the Chlorine in the ‘Diary’ SEM/EDX results is derived from the paper and/ paper contamination to the ink[55].

The ‘Diary’ ink contains the following elements that are not present in Diamine Ink,

Silicon, Aluminium, Calcium and Potassium[56]. A very searching wet chemistry analysis may find these elements in Diamine Ink as it is possible that they could be found as contaminants from the water used (this is particularly true of Calcium)[57]. However, a SEM/EDX analysis would probably not show these elements up at all as they would fall below the lower detection limit (if they were found it would only be as trace elements rather than as primary or secondary constituents)[58]. Both the Eastaugh and Leeds SEM/EDX tests found Silicon and Aluminium to be primary constituents of the ‘Diary’ ink and Calcium and Potassium as secondary elements[59]. The presence of these elements at these levels cannot be accounted for by Diamine Ink.




The Elements of Iron Gall/Ferro Gallic Inks

Iron Gall (or Ferro Gallic) inks are made from iron salts and tannin (also known as gallotanic acid and usually derived from oak galls)[60]. ‘The permanence and water-resistance of the iron and gall-nut formula made it the standard writing ink in Europe for over 700 years. Its use only started to decline in the twentieth century, when other water-proof formulas (better suited for writing on paper) became available[61].’

The basic ingredients used to manufacture Iron Gall ink would not have changed over time[62]. The following elements, Iron, Sulphur, Carbon and Oxygen can be found in any ink of this type[63]. Sodium may be present in such an ink as a constituent of Nigrosine[64] (however, as noted above, this would probably not show in a SEM/EDX analysis). Furthermore, it would be unsurprising to find all kinds of elements in Victorian Ink[65] and no elements could be said to be typical of an ink from the Victorian era[66]. Elements usually appear in ink as impurities associated with the ingredients and so if the Iron Sulphate used in the making of the ink was obtained as a by-product of making Alum, Aluminium would be present in the ink[67].

SEM/EDX of ‘Diary’ Ink and the Possibility of Contamination

It is possible that the Silicon, Aluminium, Calcium, Potassium and Sodium appear in the ink sample as containments from the ‘Diary’ paper[68]. Clay is used extensively in paper manufacture and is a form of Aluminium Silicate; depending on the variety of clay used ‘other elements can also be present, including Sodium, Calcium and Potassium[69]’. It is also the case that several paper beaching methods use Sodium Bisulphate, which contains Sodium and Sulphur[70].

The ‘Maybrick Diary’ Gas-Liquid Chromatography Analysis

Gas-Liquid Chromatography

Gas-Liquid Chromatography (GLC) is a technique for separating chemicals[71]. It is done using a gas chromatograph, which is ‘a chemical analysis instrument for separating chemicals in a complex sample’[72]. A gas chromatograph utilises a ‘flow through narrow tube known as the column through which different chemical constituents of a sample pass in a gas stream (carrier gas, mobile phase) at different rates depending on their various chemical and physical properties and their interaction with a specific column filling, called their stationary phase. As the chemicals exit the end of the column, they are detected and identified electronically[73]’. In the stationary phase the column separates different components causing each to exit at a different time[74].

Gas-Liquid Chromatography (GLC) Analysis of ‘Diary’ Ink – Results

There have been two GLC tests on the ‘Diary’ ink, both of which were looking for the chemical preservative Chloracetamide. These were carried out in 1994, the first, commissioned by Melvin Harris, was carried out by Analysis For Industry (AFI), and the second, commissioned by Shirley Harrison, was carried out by Leeds University[75].

For the AFI tests there were 3 samples, a sample of Chloracetamide, an ounce of black manuscript ink and six small ink and paper dots from the ‘Diary’[76]. The scientists first ascertained the GLC detection limit of Chloracetamide using standard solutions of Chloracetamide; they then tested the six ink and paper dots[77]. The report concluded that ‘when the six black ink dots were extracted with acetone and analyzed using gas-liquid chromatography procedures Chloracetamide was indicated to be present in the ink used[78].’

The second sets of tests were carried out at Leeds University, a first set of tests found that Chloracetamide ‘could be present in the ink’[79], however, Leeds felt that this could have been attributable to contamination and so a second series of extractions were carried out with this possibility eliminated, this time the solutions were put through in the following order, 1) methanol, 2) methanol extract of blank paper, 3) methanol extract of printed paper and 4) 100ppm standard of Chloracetamide in methanol[80]. The second time these tests were conducted (with the possibility of contamination eliminated) no Chloracetamide appeared in the ink sample. The report concluded that ‘no peaks, attributable to Chloracetamide appeared until the standard sample was injected. Thus, it appears that no acetamide is present either in the paper or printing ink used in the diary[81].’


Gas-Liquid Chromatography (GLC) ‘Diary’ Test Results and Diamine Ink

The chemical preservative Chloracetamide is present in Diamine Black Manuscript Ink (Diamine Ink)[82].

The AFI GLC found Chloracetamide in the ‘Diary’ ink and paper (combined) sample[83]. The concentration of Chloracetamide found in the AFI tests falls far below the level which would be expected of that in Diamine Ink (in fact, it is less than 10 percent of what would be expected[84]).

The Leeds GLC results found no Chloracetamide in the ‘Diary’ paper alone or ink alone samples[85].

References

AFI (1994) ‘Report on Analysis No: 409011- 19 October 1994’ Essex, AFI.

Baxendale, D (1992) ‘Report by David Baxendale’, Birmingham, Document Evidence.

CU Boulder (2007) ‘Thin Layer Chromatography – TLC’ CU Boulder Organic Chemistry Undergraduate Courses – Lab Techniques [online document.] http://orgchem.colorado.edu/hndbksupport/TLC/TLC.html  accessed 1/1/07.

Eastaugh, N. (1992) ‘A report on the analysis of: Samples from a diary purporting to be by James Maybrick – Conducted by Dr Nicholas Eastaugh – 2nd October 1992’, Middlesex (Eastaugh 1).

Eastaugh, N. (1993a) ‘Letter to Shirley Harrison, 29th March 1993’, Middlesex (Eastaugh 2).

Eastaugh, N. (1993b) ‘Ink and Paper - 16th April 1993’, Middlesex (Eastaugh 3).

Eastaugh, N. (1993c) ‘Re Diary purporting to be by James Maybrick – letter to Robert Smith 18th June 1993’ Middlesex (Eastaugh 4).

Eusman, E (of the ink corrosion website) (2007) Private correspondences, January 2007.

Forensic Evidence (2007) ‘Forensic SEM/EDX’ [online document.] http://www.forensicevidence.net/iama/sem-edxtheory.html  accessed 1/1/07.

Lane, B. (1993) The Encyclopaedia of Forensic Science, London, Headline.

Leeds University – Department of Colour Chemistry (1994a) ‘Report for The Word Team on the Analysis of the Ink used to write the “Jack the Ripper” Diaries -24th November 1994’ Leeds, Leeds University (Leeds 1).

Leeds University – Department of Colour Chemistry (1994b) ‘Presence of Chlorocetamide in ink used in diary attributed to “Jack the Ripper” – 1st December 1994’ Leeds, Leeds University (Leeds 2).

Leeds University – Department of Colour Chemistry (1994c) ‘Report for The Word Team on the Analysis of the Ink used to write the “Jack the Ripper” Diaries – 2nd December 1994’ Leeds, Leeds University (Leeds 3).

L.P.D Lab Services (2007) ‘Scanning Electron Microscopy (SEM)/EDX’ [online document.] www.lpdlabservices.co.uk/analytical_techniques/sem/index.php  accessed 1/1/07.

Rendell, K.W. (1993) ‘Report on the diary of Jack the Ripper –September 1993’, New York, The Kenneth W. Rendell Gallery Inc.

Voller, A (2007) private correspondences, January 2007.

Wikipedia (2007a) ‘Gas-Liquid Chromatography’ [online document.] http://www.en.wikipedia.org/wiki/Gas-liquid_chromatography  accessed 2/1/07.

Wikipedia (2007b) ‘Iron Gall Ink’ [online document.] http://en.wikipedia.org/wiki/Iron_gall_ink accessed 29/1/07.

Wikipedia (2007c) ‘Thin layer chromatography’ [online document.] http://en.wikipedia.org/wiki/Thin_layer_chromatography  accessed 1/1/07.



[1] Orgchem.colorado.edu

[2] Wikipedia

[3] Wikipedia

[4] Lane, pp 141

[5] Baxendale

[6] Eastaugh 1

[7] Rendell

[8] Baxendale

[9] Baxendale

[10] Baxendale

[11] Baxendale

[12] Baxendale

[13] Eastaugh 1

[14] Eastaugh 1

[15] Eastaugh 1

[16] Rendell

[17] Forensicevidence.net

[18] Forensicevidence.net

[19] Lpdlabservices.co.uk

[20] Lpdlabservices.co.uk

[21] Voller 1/07

[22] Eastaugh 1, 1992

[23] Leeds 1, 1994

[24] Eastaugh 1

[25]Eastaugh 1

[26] Eastaugh 2

[27] Eastaugh 3

[28] Leeds 1

[29] Leeds 1

[30] Leeds 3

[31] Leeds 3

[32] Leeds 3

[33] Leeds 3

[34] Leeds 3

[35] Eastaugh 2

[36] Eastaugh 2

[37] Eastaugh 2

[38] Voller 1/07, 12/06

[39] Voller 12/07, Eastaugh 1 and Leeds 1

[40] Voller 12/06

[41] Ldplabservices.co.uk

[42] Voller 1/07

[43] Leeds 1

[44] Eastaugh 1

[45] Voller 12/06

[46] Eastaugh 1, Leeds 1

[47] Voller 1/07

[48] Voller 12/06

[49] Eastaugh 1

[50] Leeds 1

[51] Voller 12/06, 1/07

[52] Voller 1/07

[53] Voller 1/07

[54] Voller 1/07

[55] Voller 1/07

[56] Voller 12/06

[57] Voller 1/07

[58] Voller 1/07

[59] Leeds 1, Eastaugh 1

[60] Wikipedia

[61] Wikipedia

[62] Eusman 1/07

[63] Voller 1/07

[64] Voller 1/07

[65] Voller 1/07

[66] Eusman 1/07

[67] Eusman 1/07

[68] Voller 1/07

[69] Voller 1/07

[70] Voller 1/07

[71] Lane, pp 140

[72] Wikipedia

[73] Wikipedia

[74] Wikipedia

[75] AFI, Leeds 2

[76] AFI

[77] AFI

[78] AFI

[79] Leeds 2

[80] Leeds 2

[81] Leeds 2

[82] Voller 1/07

[83] AFI

[84] Voller 1/07

[85] Leeds 2


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