Making Invert Sugar. How To Neutralize Acid? Is There An Upper Limit To The Cooking Temp?

[Protos]

Gentlemen, I need to make me some Inverted Sugar out of refined Beet Sugar.
I need not a Syrup, but a hard crack. I'd crush it and store it as a normal table sugar, just inverted. I'll use it not just for an adjunct but for priming as well. Cause I've got a sackful of free Beet Sugar, and need to use it up, and it is of such a quality that it gives beer a slight cidery twang even at tiny priming amounts, when raw. When inverted, it's OK however.

I've already made inverted sugar of it several times following hints published by Kirsten England, but I wasn't satisfied. The Acid added for invertion transferred into the beer and sometimes, with large sugar additions to the grist, made my beer more sour than I'd care for. I feel I need to neutralize the acid somehow. I found several sources suggesting doing that with Baking Soda, and Ron Pattinson's blog mentions using chalk for that matter in old English breweries.
Sadly, I'm totally ignorant in Chemistry and just can't calculate, for example, how much Baking Soda should I use to neutralize, say, 5 ml of 80% Lactic Acid.
So, that's my main question.

Also I have another question regarding the inversion temperature upper limit.
K. England says I shouldn't cross the 240F threshhold. I followed his suggestion, and frankly it was a PITA to keep the temperature from rising higher. On cooking forums, however, I see the chefs don't set the upper limit at all: you may cook your sugar as hot as it gets, just watch for scorching. I don't pursue creating any particular colour grade, I need just some inverted hard-crack sugar, so maybe I don't need to carefully limit my temperature as I did?

 

[Silver_Is_Money]

If I'm looking at this correctly:

A) For 80% Lactic Acid, 1 gram of Baking Soda and 1 mL of Lactic Acid should mEq balance at ~ pH 5.55.

B) For 88% Lactic Acid, 1 gram of Baking Soda and 1 mL of Lactic Acid should mEq balance at ~ pH 5.16.

To quickly and easily test/verify this you could simply add 1 mL of either of these Lactic Acid concentrations to about half a cup of good distilled water (I would not use RO water here unless it exhibits a single digit TDS reading), and then slowly mix 1 gram of baking soda into it. Stir well, then allow to cool to room temperature, then take the pH. Results as to pH may differ from my calculations because I'm presuming reactions that achieve equilibrium without any evolution of CO2 gas, such that in the real world (where there will indeed be an evolution of CO2 gas) it may be the case that each resulting final pH will be somewhat higher than my prediction.

 

[Protos]

Thanks alot, Silver_Is_Money!
That perfectly solves my confusion.
It turns out to be a very easy to remember rule of thumb: one to one!
Will add soda solution some 5 minutes before the end of the boil, after the inversion is complete.

 

[Silver_Is_Money]

Thanks alot, Silver_Is_Money!
That perfectly solves my confusion.
It turns out to be a very easy to remember rule of thumb: one to one!
Will add soda solution some 5 minutes before the end of the boil, after the inversion is complete.

Trust but verify!

 

[Silver_Is_Money]

The question which remains is:

If 5 mL of 80% Lactic Acid is added to sugar water whereby to induce inversion, at the end of the inversion process do you still have the full initial 5 mL of 80% Lactic Acid remaining in solution and waiting to be "neutralized", or will there be somewhat less active Acid remaining at this juncture?

 

[Protos]

I don't know.
I hope you'd know
It seems you are correct in your first thought, though. I've found another suggestion elsewhere to take Acid and Soda one to one. They didn't explain why, but that looks just your suggestion.

Also, I may guess the Acid quantity doesn't change significantly during the inversion process, as it sours my beer roughly the same as an equal amount of "non-invert" Acid would.
Anyway, I'd better err on the Alkaline side. Excessive acidity in a large (17%) dose of invert sugar has spoiled one of my dearest beers this May (Chevalier malt, top-cropped Verdant yeast, 19th century historical recipe followed to a tee, sanitation no worse than in a surgery room - and all that came out disappointingly tart because of the damned acid in sugar).

 

[Dr_Jeff]

When I made it, I used Cream of Tartar for the acid component.
I've read that lemon juice also works.

 

[Protos]

I tried Citric Acid once.
I think it's worse than Lactic, more intrusive flavour, so to say.
Haven't tried Cream of Tartar yet.

 

[Silver_Is_Money]

Presuming some potential for mild reaction based or temperature induced consumption/breakdown of the 5 mL of 80% Lactic Acid during the inversion process, I would likely add only 4.5 grams of Baking Soda for the first go at it.

 

[Silver_Is_Money]

5 mL of 80% Lactic Acid is a lot of acid when compared to the Citric Acid content within a wedge of Lemon. Perhaps 1/2 mL to 1 mL of 80% Lactic Acid is plenty.

 

[Silver_Is_Money]

I agree that when it comes to Beer flavor, Lactic Acid is likely to be the best choice.

 

[Protos]

I didn't take notes how much acid I used in my previous batches. I just titrated it to reach the pH of 2 in my water prior to boiling and adding sugar.
This time I will note the quantity of acid used and add equal amount of dissolved soda after the invention is complete.

 

[cire]

It is not necessary to neutralize all the acid. Ragus adjust theirs to between pH 5 and 6 before seeding with glucose for solidification. That avoids upsetting wort pH when added to the boil.

 

[Protos]

Yes, that what Silver is suggesting above: pH 5.55 when taking acid and soda 1:1.

cire, do you know, do Ragus employ temperatures above 240F for sugar invertion? Or is 240F a temperature limit set by certain chemical considerations?

 

[cire]

Yes, that what Silver is suggesting above: pH 5.55 when taking acid and soda 1:1.

cire, do you know, do Ragus employ temperatures above 240F for sugar invertion? Or is 240F a temperature limit set by certain chemical considerations?

Ragus invert at 70C, so 158 F, but at pH lower than 1.6. I would advise you might avoid that territory from personal experience. Like you I aim for pH 2, with 2:1 sugar to water, simmered until the mixture begins to color, then add more sugar, stir in, then remove heat to make syrup.

https://www.ragus.co.uk/product/brewing-sugar/
https://www.homebrewtalk.com/thread...r-favorite-recipe.472464/page-84#post-9276605

 

[Protos]

Great link to your post, thanks!
What's the maximum temperature you employ for invertion, is it 110C?

 

[cire]

I don't normally measure temperature, just thought to include whatever the meter read in those pictures.

My first serious attempts were trying to replicate what Ragus did, but at small scale there was little control and when those attempts were analyzed, about half the sugars had been destroyed.

Using the lowest setting on the smallest gas ring with constant stirring maintains simmering, the temperature determined by the sugar concentration. I assume the clear mixture color change occurs when some sugar goes beyond inversion, so is close to the end point.

As a Kg of sucrose will not fully dissolve in 500ml of water at ambient temperature, while the finished product has less water by evaporation and extra sugar by addition, when cooled to ambient, remains totally in syrup form, then a substantial proportion of sucrose must have been inverted in the process.

 

[Protos]

OK, now I think I got it. Did invertions maybe like ten times and never gave a thought to it.
For inversion, I only need some 15 to 20 minutes at 115C. Then, after the colour has changed, the invertion's done.
That means, all further cooking is not about invertion per se, but rather about modifying the colour and consistency of the inverted sugar.
Then, it doesn't really matter if I go past 115C (because the invertion's done already). I choose the temperature and length depending solely on how dark/hard I want my sugar to come out.

This time I will follow your suggestion in another thread. I don't really understand why gradual acidification is better than pre-acidifying the total water volume beforehand all the way down to 2 (as I did), but it sounds fun to try

 

[cire]

Here is the color of Ragus invert syrup.

This forms the basis of #1 Invert block. made by adding dextrose and allowing it to solidify.

#2 is made from #1 syrup, with extra color and taste from additional dark sugars (molasses), not from heat treatment.
#3 has darker sugar additions and no further heat.

High temperatures can destroy inverted sugar, as I did.

 

[Protos]

It gets even more confusing now
What is the temperature that destroys inverted sugar?

Randy Mosher recommends 150C for making Hard Crack, which suggestion I'm going to follow.
I haven't made Hard Crack yet, just syrups.

 

[cire]

I'm not an expert on sugar, just a British homebrewer who has made beer with Ragus invert sugar, the only British manufacturer of invert sugar for brewers. I have read how they make it, but cannot replicate their method.

I suggest you ask Randy Mosher what happens to sugar at 150C, and if Hard Crack is invert sugar.

 

[Protos]

Yes, that makes sense.
Also, I feel I need to dive much deeper into culinary forums. I guess, not many homebrewers make Hard Crack.
How was your sugar destroyed by high temperatures? Was it burnt/scorched?

 

[z-bob]

Is the acid actually necessary? I don't think it is, if you're patient; I think it just speeds up the process.

 

[Protos]

I read opinions that without adding acid you may simmer your syrup for hours and still have it un-inverted. Those opinions might be wrong or right, I just don't know.

 

[Misplaced_Canuck]

I'm by no means an expert, but I had decent results by using cream of tartar.

The final temperature determines the "crack level". The level of darkness was determined, in my case, by the number of water additions, so going from to cooler, to hot, repeatedly (be careful as sugar syrup can splatter).

MC

 

[cire]

I cannot find the report for my early home made sugar samples, and for the life of me I cannot recall the majority portion of the degraded sugar, a long name I'd never previously heard.

The boiling point of sugar solutions depend upon their concentration. I believe fructose will caramelize from 110C, but that could be at neutral or higher pH, while inversion is normally done at lower pH and the caramelization temperature might be higher.

Caramel is used by British brewers to add color. Timothy Taylor's Dark Mild is simply their Golden Best with caramel, but caramel isn't invert sugar.

 

[Protos]

Thanks all!
I think I've found the answers I needed on this and on confectionery forums. Stumbled there upon some really nice hints on making the inverted Hard Crack.
Invertion, it turns out, occurs at any temperature above 110. If I need an invert syrup, I should not go past 115C. If I want a Hard Crack, I just need to reach 154C. The main thing is that the total simmering time above 110C should be no less than 30 mins at pH2 for completing a full invertion.

Now I will go and make me some nice hard invert sugar.

 

[z-bob]

I found my notes from where I made dark invert sugar three years ago. I used 4 pounds of sugar, a pint of distilled water (that might be important), and 1/2 tsp of cream of tartar. I boiled it gently until the sugar dissolved (about 225°F), divided it evenly into 4 pint canning jars because I wanted each jar to contain 1 pound of sugar, topped up the jars with distilled water and sealed with canning lids, and then autoclaved them at 15 psi for an hour.

I still have a couple of jars because I don't use the stuff that often. It hasn't spoiled or tried to crystalize; if anything it has gotten slightly darker but I don't think it's even done that.

To make rock sugar you would have to open the jars and boil to the hard-crack stage. Since you probably don't want dark sugar, skip the autoclave (pressure canner), and just simmer the syrup slowly until it reaches 300°F; maybe start with a little more water. It will invert on the way there.

 

[z-bob]

Thanks all!
I think I've found the answers I needed on this and on confectionery forums. Stumbled there upon some really nice hints on making the inverted Hard Crack.
Invertion, it turns out, occurs at any temperature above 110. If I need an invert syrup, I should not go past 115C. If I want a Hard Crack, I just need to reach 154C. The main thing is that the total simmering time above 110C should be no less than 30 mins at pH2 for completing a full invertion.

Now I will go and make me some nice hard invert sugar.

If you use distilled water, you can reach pH 2 with very little acid.

 

[Protos]

Nice hint on distilled water, z-bob.
If my water is distilled, then I need less Acid to add and less Soda to neutralise it. Which is good.

 

[bwible]

Thanks all!
I think I've found the answers I needed on this and on confectionery forums. Stumbled there upon some really nice hints on making the inverted Hard Crack.
Invertion, it turns out, occurs at any temperature above 110. If I need an invert syrup, I should not go past 115C. If I want a Hard Crack, I just need to reach 154C. The main thing is that the total simmering time above 110C should be no less than 30 mins at pH2 for completing a full invertion.

Now I will go and make me some nice hard invert sugar.

I was going to suggest a candy making forum or article. Temp is everything in candy making. Temp is the difference between carmel, taffy, toffe, or hard candy,

 

[InspectorJon]

From Ragus Website:
Brewing sugar is a candy sugar made from invert sugar syrup, cane molasses, and dextrose. Producing this bespoke sugar product requires extensive sugar expertise and world-class manufacturing equipment, brought together via advanced techniques. As a result, it is only produced commercially in large inversion pans and cannot be made domestically.

So I guess we are just wasting out time.

This is what I understand so far from following this. Please correct if I got something wrong.
Inversion happens as the result of low pH, a minimum temperature and an amount of time, all three factors being variable and each affecting the outcome. Darkening happens as a result of time at a given temperature or the addition of other already darkened sugar (molasses).

So I suspect that darkening not from the introduction of molasses is the result is either caramelizing or Maillard reaction and not the inversion process. Since Maillard reactions are said to occur in a high pH environment it looks like darkening is primarily caramelization. Caramelized sugar is no as fermentable as plain sugar so to much (say a black sugar) of that might not be desirable.

Perhaps we can say that inverted brewing sugar is darkened, more flavorful inverted sugar.

 

[Protos]

So I suspect that darkening not from the introduction of molasses is the result is either caramelizing or Maillard reaction and not the inversion process.

Yes. That's right. As far as I understand now (after a massive search and read on various forums) invertion and darkening are different processes driven by different reactions. Also, I learned there's different kinds of darkening: one from Maillard reaction (which needs adding alkaline substances to the boiling sugar) and another from Caramelization, which is essentially a preliminary stage of burning and which produces different flavours.

I'm agree it requires a professional expertise to produce a real Invert Caramel Sugar, where those different processes are combined and balanced.
However, I don't think anyone trying inverting or caramelizing his sugar at home just wastes his time.
Because, empirically and practically, all the theories behind the process are proven to work in the real world, whether one understands them or not. Table sugar does really significantly change its brewing properties after invertion. It does really darken (Caramelization) when held at a proper temperature for a promer length of time, and does get a different flavour when lye is added to it (Maillard reaction).

 

[cire]

Brewing Sugars​

Brewing Sugars are produced from Raw Cane and Demerara Sugars, with colours ranging from light brown amber to dark brown, and with flavours ranging from mellow to robust treacle. They are fully inverted products; in liquid form they consist of 95% invert and 5% sucrose, while in crystalline block form they contain 75% invert, 5% sucrose and20% dextrose. Brewing Sugars are used for either economic reasons to produce the correct balance of colour and flavours, or as a nitrogen diluent to help clarify beer. They are 95% readily fermentable; lighter coloured types are used in brewing lager and pale ale, medium coloured in bitter and strong ale, and darker ones in mild ale, stouts and porters. Overuse of sugar, or using a mash with high levels of maltose, will produce thin beer. Adding dextrose or glucose can impart body and a nutty flavour. The higher the concentration of unfermented dextrose, the fruitier the beer will taste. When fermentation is complete, additional ‘priming’ sugar can be added to start secondary fermentation and increase flavour.

Caramelised Syrups​

These are produced by controlled heating of a sugar solution, at approximately 170°C. As the water evaporates, sugar molecules break down into difructose anhydride, creating compounds that contribute to flavour and a very dark brown appearance – this process is called caramelisation. Caramelised Syrups are used for colour and flavour development in dairy products, drinks, ice creams, puddings, savoury sauces and toffee. The required declaration for use in colour development is caramel E150a or Plain Caramel, and for flavour development is Caramel or Caramelised Sugar.

 

[Silver_Is_Money]

Commercial invert apparently uses strictly Hydrochloric and/or Sulfuric Acid, and appears to be carried out at temperatures in the neighborhood of only about 160-180 degrees F. Anything above that appears to merely be done whereby to induce caramelization (which is a separate subject altogether).

Since retail AMS (known to commercials as CRS) is a proprietary blend of HCl and H2SO4 it seems to be a logical acid choice. I surmise (based upon people claiming inversion success with merely a wedge of lemon) that for 1 Kg. of Sugar to be inverted, 1 mL of this acid should likely be more than adequate. Doing this in my head it appears that post-invert neutralization would require roughly 1/3 gram of Baking Soda.

AMS (CRS) is about similar to 30% Phosphoric Acid as to the latter's mEq H+ strength at a (highly specific) pH range of roughly 5.3-5.4. But since (unlike weak acids such as Phosphoric, Lactic, Citric, and Tartaric, etc...) both HCl and H2SO4 are claimed to fully dissociate at effectively any pH, AMS (CRS) presents much the same mEq acid strength at essentially any pH.

 

[Silver_Is_Money]

The above post presumes distilled water.

 

[Silver_Is_Money]

Confirmation of inversion requires that one measure the polarization of the solution before and after. It may be that much of what is presumed to be invert sugar is merely caramelized sugar.

 

[Silver_Is_Money]

I've been reading some peer reviewed articles from the late 1890's to the early 1920's on 'Wiley Online' regarding sugar inversion. The amount of acid required is such that neutralization is not considered to be required per a number of these articles, albeit that neutralization was discussed, so clearly we are not talking about a lot of requisite acidity here.

 

[Silver_Is_Money]

Back in the days of yore mentioned in my post above, when neutralization was undertaken the neutralizing substance of choice was Calcium Carbonate. Baking Soda was never mentioned. But the poor solubility of Calcium Carbonate was discussed, as was filtration.