Red color produced during Shampoo production

We make Shampoo in 500kg batches in a tank that some parts in the bottom is made of iron. Shampoo color is kind of yellow as we add orange essential oil and no other color. We then transfer it to another tank and fill the Bottles from there. Last week we made a batch and didn't transfer it to another tank. From the part which is made of iron and connected to pipe it has started producing red color in the pipe and slowly increasing day by day.

Is it contamination or iron oxide from iron part? 
If iron oxide then is it harmful in Shampoo and we should remove that part or it is ok and we can mix it with the rest of Shampoo?

Pictures are attached. 

Comments

  • Benz3neBenz3ne Member
    edited January 2021
    The red portion might be from the iron part. Have you got any laboratory contacts who can determine presence of iron oxide(s) in there? That'll give you an idea whether the equipment you're using is unsuitable or not.
    Do you mind me asking why you're not using stainless steels or coated parts?
  • @Benz3ne thanks 
    We don't have access to such laboratory that can determine it here. 

    Stainless steel tank is not available here as much as I have searched. I would have to purchase one and import from another country which with shipping and other costs it would become very expensive. 

    I would try to find a way to remove that iron part in the future. 

    Is iron oxide harmful in Shampoo? 

  • Abdullah said:
    @Benz3ne thanks 
    We don't have access to such laboratory that can determine it here. 

    Stainless steel tank is not available here as much as I have searched. I would have to purchase one and import from another country which with shipping and other costs it would become very expensive. 

    I would try to find a way to remove that iron part in the future. 

    Is iron oxide harmful in Shampoo? 

    Abdullah, search for a laboratory with ICP-MS capabilities, they should be able to determine the presence of iron oxide(s) in solution.
    Alternatively, you could try searching for qualitative tests for iron oxide(s). E.g. formation of Iron hydroxide complexes which will show as a change in colour, or formation of Prussian blue. Neither will define as accurately as laboratory methods which should be readily available. 
  • chemicalmattchemicalmatt Member, Professional Chemist
    @Abdullah, you have iron oxide there or something that was catalyzed by it - and lots of it. Can you get plastic (UDHDPE or PP) vessels and fittings where you are? As long as you don't need to heat they work fine. Getting rid of that stuff in your shampoo is another story since iron feeds bacteria really well. Throw a bunch of EDTA in there if you have any and see what happens. 
  • @Benz3ne thanks a lot
  • @chemicalmatt thanks

    These are the preservative parts
    caprylhydroxamic acid %0.1
    Glyceryl Caprylate %0.9 
    Sodium phytate %0.05 
    pH is around 5

    I have reduced the amount of sodium phytate from %0.1 to %0.05 in order to reduce the cost as it is expensive but i think it was not a good idea. I will add %0.1 edta to this batch. is that enough or should I add more?

    I will search for plastic vessels and fittings. 


  • We locally paint the oxidizable metals with this paint as it prevents the oxidation.
    The english name is "Primer based on alkyd resin and iron oxide". If i paint the iron vessels and fittings with this it will prevent the oxidation but should i do it?
    Is it safe?

    I have purred some of this Shampoo on a metal which was painted by this and haven't seen any reaction. 
  • Abdullah said:
    We locally paint the oxidizable metals with this paint as it prevents the oxidation.
    The english name is "Primer based on alkyd resin and iron oxide". If i paint the iron vessels and fittings with this it will prevent the oxidation but should i do it?
    Is it safe?

    I have purred some of this Shampoo on a metal which was painted by this and haven't seen any reaction. 
    No, you really should have fit for purpose equipment. Trying to find a temporary fix which may or may not be sufficient is not a suitable substitute for correct equipment.
  • PhilGeisPhilGeis Member, Professional formulator
    Whatever it is, you need to scrap it.  It is clearly adulterated.  And that is a pretty lame presrvative system.
  • AbdullahAbdullah Member
    edited January 2021
    PhilGeis said:
    Whatever it is, you need to scrap it.  It is clearly adulterated.  And that is a pretty lame presrvative system.
    You mean scrap only that red part or the whole batch? 

    Spectrastat G2 from Inolex has 
    %0.1 caprylhydroxamic acid
    %0.75 glyceryl caprylate
    %0.15 glycerin 
    And they say it is broad spectrum preservative.
    So at pH 5, with a chelating agent isn't that enough for Shampoo? 
  • Benz3ne said:
    Abdullah said:
    We locally paint the oxidizable metals with this paint as it prevents the oxidation.
    The english name is "Primer based on alkyd resin and iron oxide". If i paint the iron vessels and fittings with this it will prevent the oxidation but should i do it?
    Is it safe?

    I have purred some of this Shampoo on a metal which was painted by this and haven't seen any reaction. 
    No, you really should have fit for purpose equipment. Trying to find a temporary fix which may or may not be sufficient is not a suitable substitute for correct equipment.
    Thanks 
    Buying a stainless steel tank is not an option at least for now because of high price and not being available in our country because no one uses it. 
    And our Shampoo is cold process About 35°. 
  • PhilGeisPhilGeis Member, Professional formulator
    Abdullah said:
    PhilGeis said:
    Whatever it is, you need to scrap it.  It is clearly adulterated.  And that is a pretty lame presrvative system.
    You mean scrap only that red part or the whole batch? 

    Spectrastat G2 from Inolex has 
    %0.1 caprylhydroxamic acid
    %0.75 glyceryl caprylate
    %0.15 glycerin 
    And they say it is broad spectrum preservative.
    So at pH 5, with a chelating agent isn't that enough for Shampoo? 
    Yes - the whole batch. "Broad spectrum" is the marketing hype offered for every preservative and that is very weak system - esp. for a shampoo.
  • ozgirlozgirl Member, PCF student
    Spectrastat G2 is known for turning orange in the presence in iron. This is from the datasheet

    Spectrastat G2 Natural MB is compatible with most cosmetic ingredients. However, it can interact with residual iron found in some clay-type compounds (e.g., bentonite, silicates, etc.). This interaction with iron may produce a very mild orange color or color shift that is barely perceivable to the eye in most formulations. In cases where the clays are high in iron, the colored compounds may be more perceivable

  • AbdullahAbdullah Member
    edited January 2021
    @ozgirl yeah
    there is a mild orange color produced in each batch but i thought it may be from orange essential oil.
    Does this interaction reduce the effectiveness of preservative? 
  • AbdullahAbdullah Member
    edited January 2021
    PhilGeis said:
    Yes - the whole batch. "Broad spectrum" is the marketing hype offered for every preservative and that is very weak system - esp. for a shampoo.
    I did add %0.1 tetrasodium EDTA and % 0.03 citric acid as @chemic@chemicalmatt said and mixed the whole batch. pH is 5. It hasn't produced this red color again since two days. 6 people including me have used the shampoo after that and it has no irritation or smell or any negative effect.

    What if we sell this batch in discount directly to consumer? We can sell all directly to consumer to be used faster and not be stored in shops. We can sell all in one or two months. 

    Scraping 500kg Shampoo would be painful 😣 for a startup company.
  • PhilGeisPhilGeis Member, Professional formulator
    That 6 people have used it without irritation is not relevant. This is an off spec batch not made as intended.  It is adulterated and you fail in your responsibility to consumer  to do anything else than scrap the batch.  

    I sure understand it is painful to scrap the product and that you are poorly capitalized to absorb the loss.  That does not change the risk/your responsibility to consumers.   It may be as seemingly trivial as iron (alot of iron in your water?) and  the hydroxamic acid in Spectrastat (prob not - with EDTA in system).  It may not. 
    This is a test of your business practices.  What is your evaluation of quality?
  • PhilGeisPhilGeis Member, Professional formulator
    Are you using city or well water?
  • @PhilGeis thanks a lot.
    We filter the water and when enough filtered water is not available we purchase and use mineral drinking water which are being sold in Bottles.
    In this batch 50kg was mineral water.

    These two parts produce red color in a few hours when in contact with Shampoo, we have seen that when cleaning the materials. And i am sure some of the color is from this. Just want to know is there any bacteria, yeast or mold that produce red color when contaminated with?

    If not safe as Shampoo, can we use it for other things Like floor cleaning, surface cleaning, car wash, dishwashing, clothes washing or anything else?

  • PhilGeisPhilGeis Member, Professional formulator
    Filtered tap water and mineral water.   Not sure what the picture shows but it looks pretty jury rigged.  Think you're approaching cosmetic productionn in a pretty casual fashion.   The cleaning application (other than dishwash) isn't a bad idea but prob ned to rule ou bacteria or it will eventually stink. 

    Yes - Serratia marcescens famously produces a red pigment in culture and I've seen cosmetics contaminated with the bug turn red.   ozgirl also made the excellent point that iron (mineral water?) complexes with capryl hydroxamate of Spectrastat GB Natural (natural here BS - it's synthetic) to produce a red complex.   But your EDTA should compete for iron.

    In any case, you donlt know why it's red and you are resp;onsbile to prove the safety of your product and you can;t.
  • I would not throw the whole lot away, especially if it is a preservative, chelating and pH issue. Change your preservative to a well known one like Euxyl 9010, add 0.3% EDTA, not phytate and raise the pH.
    Iron oxide usually gives you a browny orange, not totally red. However, together with orange EO you will get more of a red colour.
    Does the orange EO have bergaptenes? what quality is it? maybe you need a fixative for the volatile plus a bottom note to balance out.
    Hope this helps

    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • @Dr Catherine Pratt it already has 
    %0.9 glyceryl caprylate
    %0.12 caprylhydroxamic acid
    %0.05 sodium phytate
    %0.1 tetrasodium EDTA
    %0.4 citric acid 

    I don't have Euxyl 9010 available but i have Geogard 221. By the way, wouldn't it become too much preservative and cause irritation? 

    pH is 5. What do you suggest the pH to be? 

    I don't know about bergaptenes. We use it at %0.25 and it gives a good smell. That is enough for us.
  • @Abdullah my suggestions are just for experimentation i.e. take out a sample and try these suggestions, not to put them into the whole batch.
    I have used 1 to 1.5% phytate and up to 0.5 EDTA due to packaging issues with iron. However, as I said the colour that mine usually presented were various browns.
    Geoguard is good one to try.
    I suggest changing the pH as colour is sensitive to pH as you would know. Maybe just up 1.5 to 6.5.
    Citrus Essential Oils like Bergamot contain compounds called Bergaptenes and these can play havoc within formulas turning them green even as they are very photo sensitive and if the color changes so dramatically can mean toxicity.

    So basically I am suggesting little tests taking out 50mL/test and adding my suggestions and see what you get and compare. Testing small amounts is what the formulator should be doing if you have a lot of variables and you have no idea where the problem is coming from.
    Furthermore, I would also do a microbial test to be sure as well. If you are worried about irritation, then this is something you need to spend time on.

    When you do these tests also dilute over various ratios. Adding water, then try out EDTA + Geoguard? you may have success and you have just added water and ingredients you already have in stock! Get what I mean?

    Hope this helps and I have not confused you more. Just trying to help!! Have a good one.
    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • PhilGeisPhilGeis Member, Professional formulator
    edited January 2021
    One more - you can't legally sell this as a cleaner in the US.  For that, all the ingredients must be on the TSCA inventory (https://www.epa.gov/tsca-inventory).  Further, the preservatives must be registered pesticides per EPA FIFRA - the ones mentioned are not only weak, very unlikely they're registered.  

    Think you should scrap this stuff.
  • thank you both @PhilGeis @Dr Catherine Pratt
    If i transfer this batch to another plastic tank and it didn't produce any more red color, can i be sure that it is not a preservative issue and that color was just iron oxide being produced from that iron part of tank that i have circled? I wknow that parts produce iron oxide easily in a few hours.

    Of course i will change that part soon.

  • @Dr Catherine Pratt 
    I have separated some of this batch and it doesn't produce any color and any change. The rest of the batch in this tank also doesn't produce any color change. The only part that produces red color is these two fittings which are made of iron as shown in picture and i know these parts produce iron oxide very fast. 
    My concern isn't about color, whatever color it is, it is fine for me. My concern is about contamination or being harmful to consumers.

    I have used sweet orange essential oil %0.25
  • PhilGeisPhilGeis Member, Professional formulator
    edited January 2021
    With that appropriate concern, there is no way this product should be distributed to consumers - even with compliant labeling
     21 CFR 740.10

    A cosmetic is considered misbranded if its safety has not adequately been substantiated, and it does not bear the following conspicuous statement on the PDP:

    Warning - The safety of this product has not been determined.

  • @PhilGeis thanks a lot
Sign In or Register to comment.