Contents

List of recipes Preface A brief history of the calotype Basic materials and procedures About the paper Waxing paper Marking the paper Applying solutions to paper Drying of paper negatives About making paper negatives About iodizing recipes About iodizing procedure Silver aceto-nitrate solutions Sensitizing the paper Maintenance of silver bath Darkroom Photographing Detection of exposure time Paper negative exposure disc A few words about developers The developers of paper negatives The development process Fixing Testing fixer exhaustion Neutralizing the fixer

Paper testing Checking the paper Testing paper in practice Basic processes Introduction to basic processes Guillot-Saguez process Greenlaw’s version Le Gray’s process Pelegry’s process Errors and Solutions About errors Corrections of negatives Intensification of the paper negative Reduction of intensity Retouching Pre-exposure Modern technique Photo paper as a negative Positive photographic processes Contact copies on photo paper Salted and albumen prints Binders and sensitizers Appendix Making a negative holder R&W table Removing fog Stop bath

 

Preface

The book of Calotype or paper negatives is another one of my manuals in the Historical and Alternative Photography series, which, with its reliability and facts, verified in practice, have been presenting, for more than a decade, some standard of good, modern photo manual. The contents of this book I made in the form of step-by-step, with detailed descriptions and rich pictorial material.

The topic of this book is one of the oldest procedures for the production of photographic negatives, the so-called paper negatives. These are successors of the calotype, a photographic process patented in 1841 by the English photographer W. H. F. Talbot.

The original Talbot’s process is not described in the book, because, according to Talbot’s contemporaries, the first versions of the calotype were an extremely incomplete, capricious, and almost useless to produce paper negatives. The theme of this book is a rather sophisticated technique of making paper negatives, named by Talbot’s contemporaries, as opposed to “calotype” with a simple name “paper negatives.” 

First, the book introduces the so-called Guillot-Saguez process, which was the first, much simplified, but the reliable method by which paper negatives begin to differ from Talbot’s calotype.

Next, the Greenlaw process belongs to a later period of paper negatives. Although Greenlaw’s method is a near-perfect copy of the waxed paper negatives of French photographer Gustave Le Gray, because of its effortless procedure (which is especially suitable for beginners), it deserves an essential place in this book.

The third process discussed in this book is a revolutionary process of using waxed paper negatives, invented by the French photographer Gustave Le Gray. Making negatives with this process is a bit complicated, but the results are quite good.

The fourth process of making paper negatives, called the Pelegry process, dates from the last period of paper negatives. These negatives are durable and have relatively short exposure time.

Since the book follows the idea of the step-by-step style, the reader in the initial chapters will first meet the types of paper, and how it is prepared and processed. In the next sections are descriptions of the manufacture and use of iodizing mixtures, outlines of the production and usage of a variety of paper-sensitizing solutions, and a few pages also describe the photographing techniques.  

Following this theoretical knowledge, the second part of the book describes the practical examples of the processes used by the most famous photographers mentioned above. 

Because paper negatives are quite tricky, the book also includes an extensive chapter describing errors and methods to correct them.

The next chapters speak about advanced techniques, intensification of paper negative, and reduction of intensity, and I also briefly mentioned the sometimes mandatory retouching.

At the end of the book is a chapter on the production of negatives using modern photo paper, and a full description of the creation of positive images using the then-popular methods of salt and albumen printing.

A brief history of the calotype

Writing about the history of the first photographic processes is a rather ungrateful task, as we find in old books, a considerable number of different and distorted facts. A brief presentation of the facts currenty known, however, looks something like this.

1724 German scientist Johann Heinrich Schulze (1687 – 1744) discovered that the silver compounds are sensitive to light.  He made the first photograms. He wrote a text and put it (the first negative in the world) in front of a surface, coated with the light-sensitive solution. Unfortunately, he was not able to preserve or fix the resulting images. 

1777 The Swedish chemist Carl Wilhelm Scheele (1742 – 1786) continued the experiments with silver solutions and discovered that ammonia washed away unexposed silver chloride, while exposed metallic silver was left unchanged. Scheele thus discovered the first fixer.

1802 Thomas Wedgwood (1771 – 1805) was one of the first researchers who wanted to fix the photos of the surrounding on paper. He did not succeed, but his photograms represent the first cornerstone of contemporary photography.

1816 The first photographer, Joseph Nicéphore Niépce (1765 – 1833), made his first photograph (negative) using a camera obscura and silver chloride.  Because he didn’t know how to fix the image, he began to experiment with bitumen. The first silver photo he produced was preserved until around 1860 but has since disappeared.

1823 Joseph Nicéphore Niépce produced the first photo in the world using bitumen. We can admire this image still today.

1831 Louis-Jacques-Mandé Daguerre (1787 – 1851) told his partner, the first photographer, Joseph Nicéphore Niépce, in a letter that experiments with iodine show that the sensitivity of silver to light increases tremendously with the use of iodine. Soon, with this combination, he was able to produce his first photographs with a 3-minute exposure. All he had to do was to produce a positive image and fix it.

1833 The French-Brazilian scientist, Antoine Hercule Romuald Florence (1804 – 1879), took the first photo with the help of a camera obscura and silver chloride. He was the first to use the principle of a negative and a positive image. He named his process a photographie. We can’t admire his photos anymore, but his photograms, photocopies of documents, and labels, which he fixed with urine, are today still on display.

1835 Louis-Jacques-Mandé Daguerre made a positive from the negative and also fixed that first positive photograph.

1839 French photographer Hippolyte Bayard (1801 – 1887) wanted to patent his photographic process, today so-called direct positive printing, a sort of Polaroid of the 19th century, but he failed. Academics give priority to the French photographer Louis-Jacques-Mandé Daguerre (1787 – 1851). Bayard first darkened a paper coated with salted water and silver nitrate in the sun, then he smeared potassium iodide all over it and exposed it with the camera. 

1839 French photographer Louis-Jacques-Mandé Daguerre (1787 – 1851) patented the “first” successful photographic process – the daguerreotype. With this procedure, he first produced a so-called latent image, which became visible only when exposed to mercury vapor. 

1839 A few days later, William Henry Fox Talbot (1800 – 1877) showed his negatives and photograms made with silver chloride at the Royal Institution of Great Britain in London. The exposure time was one hour or longer, as it used a fairly simple technique known today as the salt print. The salt print is a so-called “printing out” process, in which the image was not developed but became slowly visible during exposure.

1839 In April 1839, the Rev. J. B. Reade has discovered that gallic acid drastically increases the sensitivity of the paper negative.

1839 English scientist John Frederick William Herschel (1792 – 1871) discovered that sodium thiosulphate (hypo) is a much better fixer than ammonia. He informed both Daguerre and Talbot about this discovery.

1840 William Henry Fox Talbot began to develop a new process of developing a faint or almost invisible latent image used in the daguerreotype.

1841 W. H. F. Talbot patented the photographic process, in which the exposure time was shorter than in previous, salt print technique. He has begun to iodize and develop images in developer made of gallic acid. The process was named calotype or Talbotype. On the same day, as Talbot publishes his patent, always the second Bayard applies the identical procedure.

1847 Because Talbot’s process was extremely unreliable various improvements soon began to emerge. Louis-Désiré Blanquart-Evrard (1802 – 1872), in 1847, presented to the public a process in which chemicals were applied to paper by emerging or floating, not by brushes. Image quality has improved tremendously. Instead of sensitizing the negative with the so-called “gallo-nitrate of silver,” which very often destroyed paper even before it was exposed, Blanquart-Evrard in the first step treated the paper only with silver nitrate. He used gallic acid only as a developer. 

1847  Jacques-Michel Guillot-Saguez (1807-1866) fundamentally altered Talbot’s or Blanquart-Evrard’s calotype. By eliminating the first silver nitrate bath, he remarkably simplified the process. Guillot-Saguez merely iodized the paper, applied silver nitrate to it, exposed it, developed, and fixed it. More and more photographers have accepted such a simplified procedure as it has been extremely reliable. From here on, we are no longer talking about calotype but paper negatives. 

1847 Claude Félix Abel Niépce de Saint-Victor (1805 – 1870), a cousin of Joseph Nicéphore Niépce, made the first albumenized negative on glass, which significantly exceeded the quality of Talbot’s paper negatives.  

1851 French chemist Henri Victor Regnault (1810 – 1878) proposed replacing gallic acid with pyrogallic acid. At a dose of one gram per liter of water, its action is both quicker and more energetic to develop the image.

1851 Jean-Baptiste Gustave Le Gray (1820 – 1884) discovers the so-called waxed-paper, in which he waxed paper before sensitizing it. The negatives become extremely sharp for the time being, but above all, much more durable and useful even at higher temperatures. From now on, except for a few minor improvements, the development of paper natives is almost interrupted.

1851 Frederick Scott Archer (1813 – 1857) and at the same time Gustave Le Gray discovered the so-called wet plate collodion process that completely replaced daguerreotype and paper negatives. 

1884 After 1884, when the Eastman Company produced faster bromide paper for the production of negatives, the predecessor to celluloid films, paper negatives became popular again for a moment. But just for a moment. Humanity soon entered the world of celluloid films.

About the paper

The paper we use to make paper negatives is one of the most critical factors for producing quality photographs. Before doing any practical work, therefore, we must get to know its essential properties.

Basic requirements of a good paper

The paper must be free of watermarks and other inscriptions.

The structure of the paper should be free of impurities, such as darker pieces of wood or fabric. It is best to use machine-made paper.

Even paper thickness is no longer a problem nowadays since manufacturers make the new paper on extremely accurate machines. When using handmade paper, the photos are full of dark-colored spots due to the uneven thickness of the paper.

We avoid too much thin paper. Thin paper allows for much higher light transmission, but such paper is often scratched, wrinkled, or destroyed during processing. Most often, we use the so-called 70 gram (18 lb) paper.

The paper should not be too thick as it makes it more difficult to transmit light, which also increases the exposure time of a positive image. But the thicker paper also has one advantage. The positive image is less contrast and shows a lot more shades.

Nowadays, the technology of paper production has changed a lot. If papers were once quite acidic, they are now mostly acid-free. But it is better to use more acidic paper. If we use an acid-free paper, it is more probable that we need to acidify the paper (see Acidification of paper on page 77). 

Transparent or semi-transparent papers are much better for producing negatives. These reduce the time for producing a positive image.

Most fans of old photography think that the masters of photography used a few centuries ago only 100% cotton paper. But the truth is different. 150 years ago, photographers mostly used cellulose paper.

Types of paper

Although we may use almost all types of paper to make paper negatives, some types are much more useful than others.  

Art paper

To produce paper negatives, we very often use paper that we use for various artistic processes. But thinner paper, which is suitable for making paper negatives, is most often intended, not for painting, but sketching, calligraphy, and drawing. 

This paper is lightweight, and it is of an extremely high-quality internal structure and even texture. These papers are most often unproblematic in processing, but their downside is the relatively higher cost. 

Because of these positive features, for the examples in this book, we most often used one of these papers, called Canson Marker. Other popular papers are Bienfang Graphics 360, Clearprint 1000H Velum and Staedtler Mars Vellum.

Office paper

Office paper is a simple, relatively inexpensive paper of quite different qualities. We achieve the best results with slightly more expensive papers that we used for typing on classic typewriters. But when using these papers, we encounter quite a few problems. They can tear up more often, and even more often, they become entirely black during development due to their alkalic composition. 

But, as we wrote below, we can also solve these problems quite quickly.

Tracing paper

Tracing paper is designed to draw plans from which we make contact copies through various procedures. The paper is still on sale and well suited to the production of paper negatives. The advantages of this paper are the excellent transparency and the protective layer that does not require waxing. The disadvantages of this paper are two. In water, the paper likes to roll into a tube, and, when dry, often wrinkles, causing loss of sharpness on the negative.

Formats of negatives

It is almost pointless to write about the formats of paper negatives, or photographic plates since the data on them differ from book to book. We notice that the English formats are different from the American ones; these are different from the European ones. The original formats of daguerreotype plates are different from those of wet collodion, and so on.

The table below is from the 1911 Cassells Cyclopaedia Of Photography by Jones, Bernard E.

Waxing paper

The techniques used to make the paper a little more transparent and thus more like a modern photographic negative are quite a few. In this section, we described only some of the most effective procedures.

We represented the slightly modified Le Gray paper waxing technique, followed by several later techniques, such as waxing with paraffin, petroleum jelly, and a solution of glycerin and Castor oil. If we wish, we can use other means to increase transparency, but we must be careful that the agent used is not greasy, since grease may stain the final, positive image.

Another critical factor for increasing transparency is the extent to which each solution increases transparency. Some compounds are more effective than others.

In the example below, we effortlessly checked transparency. 

First, we coated pieces of paper of the same type with different solutions, placed a black tape in front, and scanned them in the scanner. We converted the image to a gray-scale image and measured the transparency of the paper using the Eyedropper tool in Adobe Photoshop.

In our case, we find that paper transparency increases the most when the paper is processed with wax (55%), followed by paraffin and Vaseline coated papers (53%) (outside the US, the word “vaseline” is used as generic for petroleum jelly). Castor oil in alcohol (42%) produces the worst transparency.

The ease of application is also essential when choosing a technique to increase paper transparency. The application of wax and paraffin is the most time consuming and the application of petroleum jelly and Castor oil the least. I prefer Vaseline because the results are almost identical to the paper waxed with beeswax or paraffin.

Waxing with beeswax

In case we want to use Le Gray’s paper negative process, we have to wax the paper before iodizing. Le Gray’s waxing process described here, which I have tailored to contemporary needs, can also be used in other processes when waxing the paper after making a negative. The waxing procedures before or after exposing the paper are therefore the same. In our example below, we have shown the waxing of an already made photo. Waxing requires white wax (1), iron (2), a thick glass plate or another flat surface slightly larger than the negative (3), and a blotting paper or paper towel without relief, wipes, or plain paper (4).

Waxing technique

Before starting work, turn on the iron, switch off steam, and set the temperature to the temperature for ironing the wool.

Put two or more sheets of blotting paper on a thick glass plate, put a paper negative on the paper, and put some pieces of wax (5) over it.

Put other clean sheets of paper on the paper negative with wax and press the hot iron several times so that the wax melts (6).

If we apply enough wax to the negative, we can see the edges of the negative (7) appearing through the blotting paper. If we use too little wax, we slightly lift the blotting paper, and we put a few more pieces of wax on the negative.

Then we remove the top sheets of paper and turn the paper negative over and check its bottom side. If we see a white area or non-waxed surface (8), we place some more pieces of wax on the non-impregnated parts of the negative and melt the wax again with the help of an iron.

When we soaked the whole negative with wax, it is time to remove the excess wax.

We remove any dirty paper from the glass or different substrates.

Then we place two clean blotting papers or sheets of paper on the glass plate. We put a paper negative on them and put two more blotting papers or a blank sheet of paper on the negative.

Now we start ironing the negatives. When paper absorbs the excess wax, we remove the paper and replace it with a clean one. If wax (9) is still visible on new clean paper, we put negative between two new sheets of paper and repeat the ironing process. Etc.

We have to store the waxed paper (10) in a dust-free room. We can use this stored paper after a few years.

Use of paraffin

Instead of bleached beeswax, we can use bleached paraffin. The results of the tests I conducted with paraffin are almost identical to the results obtained on paper waxed with beeswax. The advantage of paraffin is that it is cheaper and easier to apply. The simplest is to use paraffin from tea candles (1). We need a thick glass or some other flat plate (2), some clean blotting paper, paper towels, wipes or plain paper (3), iron (4), and a paper negative (5). 

We put two blotting papers on the glass plate, a paper negative on them, and another two blotting papers on the negative (6).

With the iron at which we set the temperature for ironing the wool, we iron out the blotting papers for two to three minutes so that they are thoroughly heated.

When the sheets of paper, the negative and the glass plate are sufficiently warmed, we coat the negative with paraffine. If the plate is warm enough, paraffin becomes liquid upon contact with the paper (7).

We turn the negative over and rub it on the other side.

We lay a blotting paper on a paper negative and iron everything so that we evenly distribute the paraffin over the surface of the negative (8).

Once we thoroughly soak the paper negative with paraffin, we remove the dirty blotting papers.

Now we put two blotting papers under and over the negative and repeat the ironing process until the blotting papers remain clean.

Increasing transparency after making a negative

Le Gray’s process of making paper negatives is different from other techniques in that Le Gray first waxed the paper and then processed it. Most other techniques for making paper negatives, however, are characterized by producing the negative first, but only after fixing, rinsing, and drying, the transparency is increased with one of the described waxing techniques.

So, to increase transparency after taking a photo, we can use the techniques just described using wax or paraffin. Still, more often in later periods, photographers have used one of the following techniques, which are equally effective but much more straightforward.

Increasing transparency with Vaseline

A somewhat simplified process for increasing transparency is the use of Vaseline, which is outside the US known as a generic name for petroleum jelly. We need the following materials and tools to work: a tube of petroleum jelly (1), iron (2), a thick glass plate (3), some blotting papers or plain but clean sheets of paper (4), and a clean cloth or paper tissue (5).   

We heat the glass plate and place two sheets of paper or blotting papers on a plate, and on them, we place a photo with the face down.

We squeeze a little petroleum jelly onto the photo and gently apply it to the paper negative (6) with a finger.

When we finished applying Vaseline on the back of the photo, we apply petroleum jelly carefully also to the front of the photo (7).

We carefully wipe off excess petroleum jelly from the image (8) with a piece of clean, very soft cloth or with a soft tissue paper.

Then we put two sheets of paper, or two blotting papers, or paper towels without relief on the paper negative.

We iron the photo with an iron, on which we set the temperature for wool ironing. In this way, the excess petroleum jelly is absorbed into the blotting papers.

If the blotting papers are wet, we replace them with clean ones. We repeatedly iron the negative until we notice that the blotting papers completely absorbed petroleum jelly.

Increasing transparency with Castor oil

The easiest way to increase the transparency of negative is the use of 25% of the Castor oil solution in alcohol. Alcohol makes it quick to dry this layer, and Castor oil, unlike other oils, does not grease paper of a positive picture. 

Unfortunately, the transparency of paper after treatment with this solution is slightly lower, but this technique was once trendy because of its simple application. For the Castor oil solution, we need the following ingredients.

• 100 ml  Ethanol 70% or higher
• 25 ml  Castor oil

We prepare the solution by mixing all the compounds (1) in a glass.

The technique of applying this solution is quite simple. We slowly apply Castor oil solution with a clean cloth to the back of the paper negative (2).

If desired, we can turn the negative over and apply the solution to its front side.

After applying this solution, ironing is unnecessary.

Marking the paper

Before we get into serious work, we need to understand some of the necessary procedures we use when working with paper. The first process is to mark one side of the paper.

Since, in most cases, we process only one side of the paper, we somehow need to know which side of the paper is front and which is back. Marking paper with a pen is undesirable for the beginners, as in many cases, they stain the whole tested paper with black color. Therefore, at least at the beginning, when we are learning the technique of paper negatives, it’s better to mark the paper side with a small notch. 

First, we cut the paper into the format and then cut a small notch in the upper-right edge of the paper in the shape of a triangle (1).

If we hold the paper so that the cut off part near the corner is always near the right thumb, we know at every moment that this is the uppermost, unprocessed side of the paper (2).

Introduction to basic processes

In this section of the book, we will describe some of the most effective, simple, and favored methods for making paper negatives. 

First, we will meet the Guillot-Saguez’s process, which has taken the calotype into a new period of paper negatives. 

Next, Greenlaw’s process represents one of the many so-called dry paper processes. It is based on Le Gray’s recipes. 

In this book, we also described one of the later versions of Le Gray’s waxed paper negatives.

Finally, we will present the process of producing unwaxed paper negatives of the French photographer Pelegry, which is an upgrade of Le Gray’s process.  

After describing the processes mentioned above that are best for beginners, follows a section on errors, with descriptions of how to get rid of problems. 

But before we get started, let me remind the reader that 99% of the errors will occur by carelessness at work. Therefore, I ask the reader to follow the instructions carefully and not change the guidelines, at least at the initial stage. 

I have thoroughly tested all the processes described in this section so that any slightly more careful reader will be able to make his first negative, even if it is unlikely to produce a quality paper negative. Quality is still mostly dependent on practice.

• We made all the tests in this chapter on Canson Marker paper. This paper is the least problematic for dealing with paper negatives. We learned about how we use other types of paper in the previous chapter (see Checking the paper on page 76 and see Testing paper in practice on page 81).
• Then we must carefully follow all instructions when making and using the solutions. It’s better to read the instructions several times, and please, do not overuse or shorten the lengthy procedures during the initial phase.
• The beginner should buy a high-quality chemical. I buy them from Sigma-Aldrich Corporation, now part of the multinational Merck. Although these chemicals are more expensive than the chemicals found in photographic shops, I never doubt their quality when working with these chemicals.
• As most chemicals are harmful to health,  I should remind the reader once again of the dangers, the emergency response, and the appropriate protection before starting work.
• Every beginner would prefer to produce the perfect photograph with the first attempt. But this is impossible due to a large number of factors that affect the creation of a paper negative.

Another requirement to avoid problems is to create a test negative to detect the right exposure time (see The step-by-step exposure of the scene on page 55). 

For starters, it is best to focus on a single arbitrary technique. Greenlaw’s process is the simplest and the best. When we choose his method, we, instead of the real photo, first make the negatives with the step-by-step exposure test. This test will detect the correct exposure time.

If the test is successful, congratulations, otherwise we will have to deal with the section that describes the most common errors and solutions (see About errors on page 106).